Sample records for maximum residue limits

  1. OECD Maximum Residue Limit Calculator

    EPA Pesticide Factsheets

    With the goal of harmonizing the calculation of maximum residue limits (MRLs) across the Organisation for Economic Cooperation and Development, the OECD has developed an MRL Calculator. View the calculator.

  2. Global Harmonization of Maximum Residue Limits for Pesticides.

    PubMed

    Ambrus, Árpád; Yang, Yong Zhen

    2016-01-13

    International trade plays an important role in national economics. The Codex Alimentarius Commission develops harmonized international food standards, guidelines, and codes of practice to protect the health of consumers and to ensure fair practices in the food trade. The Codex maximum residue limits (MRLs) elaborated by the Codex Committee on Pesticide Residues are based on the recommendations of the FAO/WHO Joint Meeting on Pesticides (JMPR). The basic principles applied currently by the JMPR for the evaluation of experimental data and related information are described together with some of the areas in which further developments are needed.

  3. Nominate a Codex MRL

    EPA Pesticide Factsheets

    The Codex Committee on Pesticide Residues (CCPR) is responsible for establishing maximum residue limits (MRLs) for pesticide residues in specific food items or in groups of food for Codex. Learn how to submit a request for a CODEX MRL.

  4. Determining the accuracy of maximum likelihood parameter estimates with colored residuals

    NASA Technical Reports Server (NTRS)

    Morelli, Eugene A.; Klein, Vladislav

    1994-01-01

    An important part of building high fidelity mathematical models based on measured data is calculating the accuracy associated with statistical estimates of the model parameters. Indeed, without some idea of the accuracy of parameter estimates, the estimates themselves have limited value. In this work, an expression based on theoretical analysis was developed to properly compute parameter accuracy measures for maximum likelihood estimates with colored residuals. This result is important because experience from the analysis of measured data reveals that the residuals from maximum likelihood estimation are almost always colored. The calculations involved can be appended to conventional maximum likelihood estimation algorithms. Simulated data runs were used to show that the parameter accuracy measures computed with this technique accurately reflect the quality of the parameter estimates from maximum likelihood estimation without the need for analysis of the output residuals in the frequency domain or heuristically determined multiplication factors. The result is general, although the application studied here is maximum likelihood estimation of aerodynamic model parameters from flight test data.

  5. Bioefficacy, residue dynamics and safety assessment of the combination fungicide trifloxystrobin 25% + tebuconazole 50%-75 WG in managing early blight of tomato (Lycopersicon esculentum Mill.).

    PubMed

    Saha, Sujoy; Purath, Ahammed Shabeer Thekkum; Jadhav, Manjusha R; Loganathan, M; Banerjee, Kaushik; Rai, A B

    2014-01-01

    This paper reports the in vitro and in vivo bioefficacy of a combination fungicide trifloxystrobin (25%) + tebuconazole (50%) against early blight disease of tomato (Lycopersicon esculentum Mill.) caused by Alternaria solani and their corresponding pre-harvest intervals (PHI) with reference to the maximum residue limits (European Union). Bioefficacy of the test fungicide combination revealed that in vitro conditions manifested the best control (75.1%) at 350 mg kg(-1) against 76.2% control under field conditions. A sample preparation method based on ethyl acetate extraction and estimation by LC-MS multiple reaction monitoring (MRM) was validated in tomato fruits at 0.01 mg/kg and dissipation studies were conducted in field at single and double doses. The residues of both the compounds on all the sampling days were below the European Union maximum residue limits (EU-MRLs) and the maximum permissible intakes (MPIs) were calculated on the basis of prescribed acceptable daily intake (ADI). The combined bioefficacy and residue dynamics information will support label-claim of this fungicide combination for the management of early blight in tomato.

  6. Residues and dissipation kinetics of carbendazim and diethofencarb in tomato (Lycopersicon esculentum Mill.) and intake risk assessment.

    PubMed

    Li, Huidong; du, Hongxia; Fang, Liping; Dong, Zhan; Guan, Shuai; Fan, Wenjing; Chen, Zilei

    2016-06-01

    Dissipation behaviors and residues of carbendazim and diethofencarb in combination in tomato were investigated. The half-lives were 2.1-3.4 days for carbendazim, and 1.8-3.2 days for diethofencarb at a dose of 1.5 times of the recommended dosage. The residues of carbendazim and diethofencarb were below the maximum residue limits (MRLs) in China one day after application of the combination. The ultimate residues were significantly lower than the maximum permissible intake (MPI) in China at the recommended high dose for both child and adult. The values of the maximum dietary exposure for carbendazim and diethofencarb were 0.26 and 0.27 mg per person per day, respectively. The theoretical maximum daily intake (TMDI) values for carbendazim and diethofencarb were 1.5 and 0.5 mg/day, respectively. The dietary exposure was lower than the MPI, which indicates the harvested tomato samples under the experimental conditions (open field) are safe for human consumption at the recommended high dosage of the wettable powder. Copyright © 2016 Elsevier Inc. All rights reserved.

  7. 40 CFR 180.422 - Tralomethrin; tolerances for residues.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...-handling establishments, including food service, manufacturing, and processing establishments, such as... shall be limited to a maximum of 0.06 percent active ingredient. Contamination of food and food-contact...) PESTICIDE PROGRAMS TOLERANCES AND EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Specific Tolerances...

  8. Pesticide Tolerances

    EPA Pesticide Factsheets

    EPA regulates pesticides used to protect crops and sets limits on the amount of pesticide remaining in or on foods in the U.S. The limits on pesticides on foods are called tolerances in the U.S. (maximum residue limits (MRLs) in many other countries).

  9. De-contamination of pesticide residues in food by ionizing radiation

    NASA Astrophysics Data System (ADS)

    Basfar, Ahmed A.; Mohamed, Khaled A.; Al-Saqer, Omar A.

    2012-04-01

    The role of gamma irradiation on removal of pesticides in aqueous solutions or in vegetables and fruits was investigated. Radiation - induced decontamination of pesticides is generally greater in aqueous solutions than in selected vegetables and fruits. Residues of malathion (0.5 ppm in potatoes, 8 ppm in onions and dates), pirimiphos-methyl (1 ppm in onions and grapes) and cypermethrin (0.05 ppm in potatoes and 0.1 ppm in onions) were not reduced to below maximum residue limits (MRLs) for irradiation doses up to 1 kGy. The same trend was observed when irradiation was performed for grapes fortified with malathion (8 ppm) and cypermethrin (2 ppm) for absorbed doses up to 2 kGy. Ionizing radiation reduced the residues of pirimiphos-methyl (0.05 ppm in potatoes at1 kGy, 1 ppm in grapes at 2 kGy and 0.1 ppm in dates at1 kGy), malathion (8 ppm in grapes at 7 kGy) and cypermethrin (2 ppm in grapes at 7 kGy) to below maximum residue limits (MRLs).

  10. Residual determination and risk assessment of buprofezin in plum (Prunus domestica) grown in open-field conditions following the application of three different formulations.

    PubMed

    Kabir, Md Humayun; Abd El-Aty, A M; Kim, Sung-Woo; Lee, Han Sol; Rahman, Md Musfiqur; Lee, Young-Jun; Chung, Hyung Suk; Lieu, Truong; Choi, Jeong-Heui; Shin, Ho-Chul; Im, Geon-Jae; Hong, Su Myeong; Shim, Jae-Han

    2016-11-01

    This study was conducted to characterize the residual level and perform a risk assessment on buprofezin formulated as an emulsifiable concentrate, wettable powder, and suspension concentrate over various treatment schedules in plum (Prunus domestica). The samples were extracted with an AOAC quick, easy, cheap, effective, rugged, and safe, 'QuEChERS', method after major modifications. As intrinsic interferences were observed in blank plum samples following dispersive-solid phase extraction (consisting of primary secondary amine and C 18 sorbents), amino cartridges were used for solid-phase extraction. Analysis was carried out using liquid chromatography with diode array detection and confirmed by liquid chromatography-tandem mass spectrometry. The method showed excellent linearity with determination coefficient (R 2  = 1) and satisfactory recoveries (at two spiking levels, 0.5 and 2.5 mg/kg) between 90.98 and 94.74% with relative standard deviation (RSD) ≤8%. The limit of quantification (0.05 mg/kg) was considerably lower than the maximum residue limit (2 mg/kg) set by the Codex Alimentarius. Absolute residue levels for emulsifiable concentrates were highest, perhaps owing to the dilution rate and adjuvant. Notably, all formulation residues were lower than the maximum residue limit, and safety data proved that the fruits are safe for consumers. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  11. Residues in Beeswax: A Health Risk for the Consumer of Honey and Beeswax?

    PubMed

    Wilmart, Olivier; Legrève, Anne; Scippo, Marie-Louise; Reybroeck, Wim; Urbain, Bruno; de Graaf, Dirk C; Steurbaut, Walter; Delahaut, Philippe; Gustin, Pascal; Nguyen, Bach Kim; Saegerman, Claude

    2016-11-09

    A scenario analysis in regard to the risk of chronic exposure of consumers to residues through the consumption of contaminated honey and beeswax was conducted. Twenty-two plant protection products and veterinary substances of which residues have already been detected in beeswax in Europe were selected. The potential chronic exposure was assessed by applying a worst-case scenario based on the addition of a "maximum" daily intake through the consumption of honey and beeswax to the theoretical maximum daily intake through other foodstuffs. For each residue, the total exposure was finally compared to the acceptable daily intake. It is concluded that the food consumption of honey and beeswax contaminated with these residues considered separately does not compromise the consumer's health, provided proposed action limits are met. In regard to residues of flumethrin in honey and in beeswax, "zero tolerance" should be applied.

  12. Dissipation of Flonicamid in Honeysuckle and Its Transfer during Brewing Process.

    PubMed

    Wang, Yujie; Xue, Jian; Jin, Hongyu; Ma, Shuangcheng

    2017-05-01

    The dissipation of flonicamid in Honeysuckle and transfer pattern from Honeysuckle to its tea infusion were investigated. Flonicamid was applied on Honeysuckle crop at two dosages, 60 g of active gradient per hectare (g a.i. hm -2 ) and 180 g a.i. hm -2 (recommended and triple the recommended) in Fenqiu, Henan Province in 2015 and 2016. Gas Chromatography-Electron Capture Detector (GC-ECD) detection methods were developed for the analysis of flonicamid residues in honeysuckles and its infusion. The recoveries in both honeysuckles and its infusion ranged from 81.5 to 101.7% with relative standard deviations (RSDs) of 3.2-9.1%. The dissipations of flonicamid in Honeysuckle were found to follow the first order kinetics with half-life ranging between 2.8 and 3.2 d. After recommended dose pesticide application, contents of flonicamid residues were lower than theoretical maximum residue limit (tMRL). Flonicamid residues can easily transfer from Honeysuckle to its tea infusion and transfer rates of flonicamid decrease with the brewing temperature reduction or the brewing times increase. These results are helpful to establish maximum residue limit and develop guidance on the appropriate and secure use of flonicamid in Honeysuckle.

  13. Pesticide Residues in Food: Attitudes, Beliefs, and Misconceptions among Conventional and Organic Consumers.

    PubMed

    Koch, Severine; Epp, Astrid; Lohmann, Mark; Böl, Gaby-Fleur

    2017-12-01

    Pesticide use and pesticide residues in foods have been the subject of controversial public discussions and media coverage in Germany. Against this background, a better understanding of public risk perceptions is needed to promote efficient public health communication. To this end, this study captures the German public's perception of pesticide residues in foods. A representative sample of the population aged 14 years and older (n = 1,004) was surveyed via computer-assisted telephone interviewing on their attitudes and knowledge with regard to pesticide residues. Based on questions regarding their typical consumer behavior, respondents were classified into conventional and organic consumers to identify differences as well as similarities between these two consumer types. As assessed with an open-ended question, both organic and conventional consumers viewed pesticides, chemicals, and toxins as the greatest threats to food quality and safety. Evaluating the risks and benefits of pesticide use, more than two-thirds of organic consumers (70%) rated the risks as greater than the benefits, compared with just over one-half of conventional consumers (53%). Concern about the detection of pesticide residues in the food chain and bodily fluids was significantly higher among organic compared with conventional consumers. Only a minority of respondents was aware that legal limits for pesticide residues (referred to as maximum residue levels) exist, with 69% of organic and 61% of conventional consumers believing that the presence of pesticide residues in foods is generally not permitted. A lack of awareness of maximum residue levels was associated with heightened levels of concern about pesticide residues. Finally, general exposure to media reporting on pesticide residues was associated with more frequent knowledge of legal limits for pesticide residues, whereas actively seeking information on pesticide residues was not. The possible mechanisms underlying these findings are discussed.

  14. Risk assessment and monitoring of dinotefuran and its metabolites for Chinese consumption of apples.

    PubMed

    Yu, Weiwei; Huang, Min; Chen, Jiaojiao; Wu, Sizhuo; Zheng, Kunming; Zeng, Song; Zhang, Kankan; Hu, Deyu

    2017-09-26

    Residues of dinotefuran and its metabolites, 1-methyl-3-(tetrahydro-3-furylmethyl)urea (UF) and 1-methyl-3-(tetrahydro-3-furylmethyl)guanidine (DN), in apple were investigated using a "QuEChERS" (quick, easy, cheap, effective, rugged, safe) pretreatment and liquid chromatography-tandem mass spectrometry. Limits of detection (LODs) and quantification (LOQs) of dinotefuran, UF, and DN in apples were 0.011-0.960 and 0.037-3.200 μg/kg, respectively. The average recoveries of dinotefuran, UF, and DN in apple ranged from 70.0 to 83.6% with relative standard deviations less than 13%. A formulation of 20% water-dispersible dinotefuran granules was sprayed at 1-1.5-fold the recommended dose 3-4 times on apple trees. Total terminal residues of dinotefuran in apple were less than 2 mg/kg, which is the maximum residue limit (MRL) set by Japan. When following the recommended application guidelines, dinotefuran is unlikely to present significant health concerns to the Chinese population because the risk quotient (RQ) is less than 100%. This work could provide guidance for the safe use of dinotefuran and serve as a reference for the establishment of a maximum residue limit of dinotefuran in apple in China.

  15. Ivermectin residues in squab.

    PubMed

    Bennett, D C; Cheng, K M

    2012-11-01

    No drugs have been approved for the treatment of parasitic nematodes in pigeons, but ivermectin, a broad-spectrum endectocide, has been used extra-label by prescription. Producers currently allow for a 2-wk withdrawal time before marketing squabs. However, because its use is extra-label there is no legal maximum residue limit for ivermectin in squab meat. The purpose of this study was to examine the depletion of ivermectin (passed by the parents to the squabs) from the tissues of squab. Adult pigeons brooding squab were treated with ivermectin in their drinking water (3.3 µg/mL) for 3 d. After dosing the parents, the ivermectin concentration of the breast meat and liver of squabs was found to be greater than the maximum residual limits established for livestock, indicating that ivermectin was transferred from the parents to the squabs. However, ivermectin was not detected in either the breast meat or the livers of squabs 1 wk after dosing. These results indicate that there is a rapid decline in tissue levels of ivermectin in squab.

  16. Dissipation and residue of myclobutanil in lychee.

    PubMed

    Liu, Yanping; Sun, Haibin; Liu, Fengmao; Wang, Siwei

    2012-06-01

    The dissipation and residue of myclobutanil in lychee under field conditions were studied. To determine myclobutanil residue in samples, an analytical method with a florisil column clean-up and detected by gas chromatography-electron capture detector (GC-ECD) was developed. Recoveries were found in the range of 83.24 %-89.00 % with relative standard deviations of 2.67 %-9.88 %. This method was successfully applied to analyze the dissipation and residue of myclobutanil in lychee in Guangdong and Guangxi Province, China. The half lives in lychee were from 2.2 to 3.4 days. The residues of myclobutanil in lychee flesh were all below the limit of quantification (LOQ) value (0.01 mg/kg), and most of the residues were concentrated in the peel. The terminal residues of myclobutanil were all bellow the maximum residue limit (MRL) value set by European Union (EU) (0.02 mg/kg). Hence it was safe for the use of this pesticide and the results also could give a reference for MRL setting of myclobutanil in lychee in China.

  17. International Harmonization of Food Safety Assessment of Pesticide Residues.

    PubMed

    Ambrus, Árpád

    2016-01-13

    This paper summarizes the development of principles and methods applied within the program of the FAO/WHO Codex Alimentarius during the past 50 years for the safety assessment of pesticide residues in food and feed and establishing maximum residue limits (MRLs) to promote free international trade and assure the safety of consumers. The role of major international organizations in this process, the FAO capacity building activities, and some problematic areas that require special attention are briefly described.

  18. LC-MS/MS measurement of ampicillin residue in chicken tissues at 2 days after in-feed administration

    PubMed Central

    HAMAMOTO, Kouko; MIZUNO, Yasuharu

    2017-01-01

    We assessed ampicillin (ABPC) concentrations of liver, kidney and skin at a 2-day withdrawal period in ten male and ten female White Leghorn chickens fed the diet containing ABPC (ABPC medicated feed 40 mg/kg body weight/day) for a week. The ABPC residues were measured with liquid chromatography–tandem mass spectrometry and the mean recoveries and quantitation limits ranged from 93.0% to 102.7% and from 0.1 to 1.4 ng/g, respectively. The residual ABPC concentrations were ≤7.82 ng/g for the skin and ≤0.64 ng/g for the kidney, suggesting below the Japanese provisional maximum residue limits. These results revealed that the analytical method is developed for residue ABPC and that the withdrawal period is appropriate. PMID:28190817

  19. Statistical Techniques to Analyze Pesticide Data Program Food Residue Observations.

    PubMed

    Szarka, Arpad Z; Hayworth, Carol G; Ramanarayanan, Tharacad S; Joseph, Robert S I

    2018-06-26

    The U.S. EPA conducts dietary-risk assessments to ensure that levels of pesticides on food in the U.S. food supply are safe. Often these assessments utilize conservative residue estimates, maximum residue levels (MRLs), and a high-end estimate derived from registrant-generated field-trial data sets. A more realistic estimate of consumers' pesticide exposure from food may be obtained by utilizing residues from food-monitoring programs, such as the Pesticide Data Program (PDP) of the U.S. Department of Agriculture. A substantial portion of food-residue concentrations in PDP monitoring programs are below the limits of detection (left-censored), which makes the comparison of regulatory-field-trial and PDP residue levels difficult. In this paper, we present a novel adaption of established statistical techniques, the Kaplan-Meier estimator (K-M), the robust regression on ordered statistic (ROS), and the maximum-likelihood estimator (MLE), to quantify the pesticide-residue concentrations in the presence of heavily censored data sets. The examined statistical approaches include the most commonly used parametric and nonparametric methods for handling left-censored data that have been used in the fields of medical and environmental sciences. This work presents a case study in which data of thiamethoxam residue on bell pepper generated from registrant field trials were compared with PDP-monitoring residue values. The results from the statistical techniques were evaluated and compared with commonly used simple substitution methods for the determination of summary statistics. It was found that the maximum-likelihood estimator (MLE) is the most appropriate statistical method to analyze this residue data set. Using the MLE technique, the data analyses showed that the median and mean PDP bell pepper residue levels were approximately 19 and 7 times lower, respectively, than the corresponding statistics of the field-trial residues.

  20. Evaluation of certain veterinary drug residues in food. Seventy-eighth report of the Joint FAO/WHO Expert Committee on Food Additives.

    PubMed

    2014-01-01

    This report represents the conclusions of a Joint FAO/WHO Expert Committee convened to evaluate the safety of residues of certain veterinary drugs in food and to recommend maximum levels for such residues of food. The first part of the report considers general principles regarding the evaluation of residues of veterinary drugs within the terms of reference of the Joint FAO/WHO Expert Committee on Food Additives (JECFA), including extrapolation of maximum residue limits (MRLs) to minor species, MRLs for veterinary drug residues in honey, MRLs relating to fish and fish species, dietary exposure assessment methodologies, the decision-tree approach to the evaluation of residues of veterinary drugs and guidance for JECFA experts. Summaries follow of the Committee's evaluations of toxicology and residue data on a variety of veterinary drugs: two anthelminthic agents (derquantel, monepantel), three antiparasitic agents (emanectin benzoate, ivermectin, lasalocid sodium), one antibacterial, antifungal and anthelminthic agent (gentian violet), a production aid (recombinant bovine somatotropins) and an adrenoceptor agonist and growth promoter (zilpaterol hydorchloride). Annexed to the report is a summary of the Committee's recommendations on these drugs, including acceptable daily intakes (ADIs)) and proposed MRLs.

  1. Probabilistic Estimation of Critical Flaw Sizes in the Primary Structure Welds of the Ares I-X Launch Vehicle

    NASA Technical Reports Server (NTRS)

    Pai, Shantaram S.; Hoge, Peter A.; Patel, B. M.; Nagpal, Vinod K.

    2009-01-01

    The primary structure of the Ares I-X Upper Stage Simulator (USS) launch vehicle is constructed of welded mild steel plates. There is some concern over the possibility of structural failure due to welding flaws. It was considered critical to quantify the impact of uncertainties in residual stress, material porosity, applied loads, and material and crack growth properties on the reliability of the welds during its pre-flight and flight. A criterion--an existing maximum size crack at the weld toe must be smaller than the maximum allowable flaw size--was established to estimate the reliability of the welds. A spectrum of maximum allowable flaw sizes was developed for different possible combinations of all of the above listed variables by performing probabilistic crack growth analyses using the ANSYS finite element analysis code in conjunction with the NASGRO crack growth code. Two alternative methods were used to account for residual stresses: (1) The mean residual stress was assumed to be 41 ksi and a limit was set on the net section flow stress during crack propagation. The critical flaw size was determined by parametrically increasing the initial flaw size and detecting if this limit was exceeded during four complete flight cycles, and (2) The mean residual stress was assumed to be 49.6 ksi (the parent material s yield strength) and the net section flow stress limit was ignored. The critical flaw size was determined by parametrically increasing the initial flaw size and detecting if catastrophic crack growth occurred during four complete flight cycles. Both surface-crack models and through-crack models were utilized to characterize cracks in the weld toe.

  2. [Scientific basis in the setting of residue limits for veterinary drugs in food of animal origin taking into account the presence of their metabolites].

    PubMed

    Mitsumori, K

    1993-01-01

    Maximum residue level (MRL) for veterinary drugs in food of animal origin has been proposed by FAO/WHO, as a new evaluation procedure taking into account the presence of metabolites for the regulation of veterinary drug residues. The MRL is the maximum concentration of residue resulting from the use of a veterinary drug that is recommended to be legally permitted as acceptable in a food. It is established from the Acceptable Daily Intake (ADI) obtained from the data of toxicological studies, the residue concentration of the drug when used according to good practice in the use of veterinary drugs, and the lowest level consistent with the practical analytical methods available for routine residue analysis. Among the veterinary drugs, some chemicals contain a large amount of bound residues that are neither extractable from tissues by the analytical method identical with that used in parent chemicals. Especially, the bioavailable residues which are probably absorbed when the food is ingested are of great toxicological concern. In this case, the FAO/WHO recommends that the MRL can be established after the calculation of daily intake of residues of toxicological concern by the addition of both the extractable and bioavailable bound residues.

  3. Photoacoustic Spectroscopy as a Non-destructive Tool for Quantification of Pesticide Residue in Apple Cuticle

    NASA Astrophysics Data System (ADS)

    Liu, Lixian; Wang, Yafei; Gao, Chunming; Huan, Huiting; Zhao, Binxing; Yan, Laijun

    2015-06-01

    Photoacoustic spectroscopy (PAS), the non-destructive method to detect residue of dimethyl-dichloro-vinyl-phosphate (DDVP) pesticide in a cuticle of apple, is described. After constructing the PA experimental setup and identifying three characteristic peaks of DDVP in the near ultraviolet region, the PA spectra of an apple cuticle contaminated with DDVP were collected. The artificial neural network method was then applied to analyze data quantitatively. The results show a correlation coefficient exceeding 0.99 and a detection limit of 0.2 ppm, which is within the national food safety standard for maximum residue limits for pesticides in food (GB 2763-2012). This fact and the non-destructive character of PAS make the approach promising for detection of pesticide residue in fruits.

  4. Dissipation of chlorantraniliprole in tomato fruits and soil.

    PubMed

    Malhat, Farag; Abdallah, Hend; Hegazy, Islam

    2012-03-01

    The main objective of this study was to understand the residue and persistence behaviour of new insecticide chlorantraniliprole in tomato fruit and soil samples. Its residue was analyzed by HPLC and it dissipated in tomato fruit and soil following first order kinetics. The results showed half life (t(1/2)) value of 3.30 and 3.66 days for chlorantraniliprole in tomato fruit and soil, respectively. According to maximum residue limit (MRL) the pre-harvest interval (PHI) of chlorantraniliprole on tomato was 8-days after the treatment.

  5. Multi-residue analysis of pesticides, plant hormones, veterinary drugs and mycotoxins using HILIC chromatography - MS/MS in various food matrices.

    PubMed

    Danezis, G P; Anagnostopoulos, C J; Liapis, K; Koupparis, M A

    2016-10-26

    One of the recent trends in Analytical Chemistry is the development of economic, quick and easy hyphenated methods to be used in a field that includes analytes of different classes and physicochemical properties. In this work a multi-residue method was developed for the simultaneous determination of 28 xenobiotics (polar and hydrophilic) using hydrophilic interaction liquid chromatography technique (HILIC) coupled with triple quadrupole mass spectrometry (LC-MS/MS) technology. The scope of the method includes plant growth regulators (chlormequat, daminozide, diquat, maleic hydrazide, mepiquat, paraquat), pesticides (cyromazine, the metabolite of the fungicide propineb PTU (propylenethiourea), amitrole), various multiclass antibiotics (tetracyclines, sulfonamides quinolones, kasugamycin and mycotoxins (aflatoxin B1, B2, fumonisin B1 and ochratoxin A). Isolation of the analytes from the matrix was achieved with a fast and effective technique. The validation of the multi-residue method was performed at the levels: 10 μg/kg and 100 μg/kg in the following representative substrates: fruits-vegetables (apples, apricots, lettuce and onions), cereals and pulses (flour and chickpeas), animal products (milk and meat) and cereal based baby foods. The method was validated taking into consideration EU guidelines and showed acceptable linearity (r ≥ 0.99), accuracy with recoveries between 70 and 120% and precision with RSD ≤ 20% for the majority of the analytes studied. For the analytes that presented accuracy and precision values outside the acceptable limits the method still is able to serve as a semi-quantitative method. The matrix effect, the limits of detection and quantification were also estimated and compared with the current EU MRLs (Maximum Residue Levels) and FAO/WHO MLs (Maximum Levels) or CXLs (Codex Maximum Residue Limits). The combined and expanded uncertainty of the method for each analyte per substrate, was also estimated. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Pesticide residue evaluation in major staple food items of Ethiopia using the QuEChERS method: a case study from the Jimma Zone.

    PubMed

    Mekonen, Seblework; Ambelu, Argaw; Spanoghe, Pieter

    2014-06-01

    Samples of maize, teff, red pepper, and coffee (green bean and coffee bean with pulp) were collected from a local market in the Jimma Zone, Ethiopia. Samples were analyzed for the occurrence of cypermethrin, permethrin, deltamethrin, chlorpyrifos ethyl, DTT and its metabolites, and endosulfan (α, β). In the analytical procedure, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction methodology with dispersive solid phase extraction clean up (d-SPE) technique was applied. Validation of the QuEChERS method was satisfactory. Recovery percentages of most pesticides were in the range of 70% to 120%, with good repeatability (%relative standard deviation < 20). The limit of detection and limit of quantification varied between 0.001 µg/g and 0.092 µg/g and between 0.002 µg/g and 0.307 µg/g, respectively. The main pesticides detected were DDT, endosulfan, cypermethrin, and permethrin. All of the pesticides analyzed were detected in red pepper and green coffee bean. Residues of DDT in coffee pulp significantly differed (p < 0.01) from other food items except for red pepper. The concentration of pesticides in the food items varied from 0.011 mg/kg to 1.115 mg/kg. All food items contained 1 or more pesticides. Two-thirds of the samples had residues below corresponding maximum residue limits, and the remaining one-third of samples were above the maximum residue limits. These results indicate the need for a good pesticide monitoring program to evaluate consumer risk for the Ethiopian people. © 2014 SETAC.

  7. Beta agonists in livestock feed: status, health concerns, and international trade.

    PubMed

    Centner, T J; Alvey, J C; Stelzleni, A M

    2014-09-01

    Since the U.S. Food and Drug Administration approved ractopamine hydrochloride and zilpaterol hydrochloride in animal feeds, usage of those compounds has been a topic of worldwide debate. Ractopamine and zilpaterol are β-adrenergic agonists used as veterinary drugs to increase weight gain in certain animals raised for food. The Joint FAO/WHO Expert Committee on Food Additives (JECFA) established maximum residue limits for ractopamine, which were adopted by the Codex Alimentarius Commission (Codex). No maximum residue limits for zilpaterol have been adopted by JECFA, and new reports of animal mobility issues confront the use of this feed additive. However, many countries disagree with the Codex standards and are restricting or banning meat products containing β agonists. The bans by major importers of U.S. meat products have prompted some to advocate that the United States use the World Trade Organization dispute settlement body. This paper looks at the developments to provide a fuller accounting of what the issues may mean to U.S. firms selling meat products containing residues of β agonists.

  8. Liquid chromatography-electrospray ionization tandem mass spectrometry and dynamic multiple reaction monitoring method for determining multiple pesticide residues in tomato.

    PubMed

    Andrade, G C R M; Monteiro, S H; Francisco, J G; Figueiredo, L A; Botelho, R G; Tornisielo, V L

    2015-05-15

    A quick and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method, using dynamic multiple reaction monitoring and a 1.8-μm particle size analytical column, was developed to determine 57 pesticides in tomato in a 13-min run. QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for samples preparations and validations was carried out in compliance with EU SANCO guidelines. The method was applied to 58 tomato samples. More than 84% of the compounds investigated showed limits of detection equal to or lower than 5 mg kg(-1). A mild (<20%), medium (20-50%), and strong (>50%) matrix effect was observed for 72%, 25%, and 3% of the pesticides studied, respectively. Eighty-one percent of the pesticides showed recoveries ranging between 70% and 120%. Twelve pesticides were detected in 35 samples, all below the maximum residue levels permitted in the Brazilian legislation; 15 samples exceeded the maximum residue levels established by the EU legislation for methamidophos; and 10 exceeded limits for acephate and four for bromuconazole. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Determination of benazolin-ethyl residues in soil and rape seed by SPE clean-up and GC with electron capture detection.

    PubMed

    Liu, Xiaolu; Yang, Tao; Hu, Jiye

    2013-01-01

    A method has been developed and established for residue determination of benazolin-ethyl in soil and rape seed samples by gas chromatography with electron capture detection (GC-ECD). Limits of quantification of the method are 0.005 mg/kg for both soil and rape seed, which are sufficiently below the maximum residue limit, and the limit of detection is 0.0023 ng. The average recoveries of the analyte range from 85.89 to 105.84% with relative standard deviations (coefficient of variation) less than 5.53% at the three spike levels (0.005, 0.1 and 0.5 mg/kg). The half-life of benazolin-ethyl in soil from the experimental field is 4.62 days. The final residues of benazolin-ethyl in soil and rape seed samples are lower than 0.005 mg/kg at harvest time. Direct confirmation of the analyte in real samples is achieved by GC-mass spectrometry. It is demonstrated that the proposed method is simple, rapid and efficient, and reliable to detect benazolin-ethyl residues in soil and rape seed samples.

  10. Effect of ferrous sulfate and nitrohumic acid neutralization on the leaching of metals from a combined bauxite residue.

    PubMed

    Ren, Jie; Liu, Jidong; Chen, Juan; Liu, Xiaolian; Li, Fasheng; Du, Ping

    2017-04-01

    Bauxite residue neutralization is intended to open opportunities for revegetation and reuse of the residue. Ferrous sulfate (FS) and nitrohumic acid (NA) were two kinds of materials studied for pH reduction of the residue from 10.6 to 8.3 and 8.1, respectively. The effects of FS and NA on the leaching of metals from a combined bauxite residue were investigated by using sequential and multiple extraction procedures. Neutralization with FS and NA restricted the leaching of Al, V, and Pb from the residue but promoted the leaching of Fe, Cu, Mn, and Ni, consistent with the changes in the potentially mobile fractions. With the exceptions of Pb and Ni, leaching of metals increased during a 10-day extraction period. However, the maximum leaching of Al, V, Pb, Fe, Cu, Mn, and Ni from neutralized bauxite residue were 0.46 mg/L, 59.3, 12.9, 167, 95.3, 15.5, and 14.5 μg/L, respectively, which were under the corresponding limits in the National Standard (GB/T 14848-93). Although it is necessary to consider the continued leaching of metals during neutralization, both maximum and accumulation leaching concentrations of metals from a combined bauxite residue were too low to pose a potential environmental risk.

  11. Evaluation of pesticide residues in fruits and vegetables from Algeria.

    PubMed

    Mebdoua, Samira; Lazali, Mohamed; Ounane, Sidi Mohamed; Tellah, Sihem; Nabi, Fahima; Ounane, Ghania

    2017-06-01

    A total of 160 samples of 13 types of fresh fruits and vegetables from domestic production and import were analysed to detect the presence of pesticide residues. Analysis was performed by multi-residual extraction followed by gas chromatography-mass spectrometry. In 42.5% of the tested samples, no residues were found and 12.5% of samples contained pesticide residues above maximum residue limits. Risk assessment for long-term exposure was done for all pesticides detected in this study. Except chlorpyrifos and lambda-cyhalothrin, exposure to pesticides from vegetables and fruits was below 1% of the acceptable daily intake. Short-term exposure assessment revealed that in seven pesticide/commodity combinations, including three pesticides (chlorpyrifos, deltamethrin and lambda-cyhalothrin), the acute reference dose had been exceeded.

  12. Validation of the LacTek test applied to spiked extracts of tissue samples: determination of performance characteristics.

    PubMed

    Mitchell, J M; Yee, A J; McNab, W B; Griffiths, M W; McEwen, S A

    1999-01-01

    LacTek tests are competitive enzyme-linked immunosorbent assays intended for rapid detection of antimicrobial residues in bovine milk. In this study, the LacTek test protocol was modified for use with extracts of bovine tissue to detect beta-lactam, tetracycline, and sulfamethazine residues. Test performance characteristics--precision, accuracy, ruggedness, practicability, and analytical specificity and sensitivity--were investigated. Results suggest that LacTek tests can be easily adapted to detect antimicrobial residues in extracts of lean ground beef. However, positive samples may not contain residues at violative concentrations (i.e., Canadian maximum residue limits), and therefore, additional analysis would be required for final confirmation and quantitation (e.g., chromatography).

  13. Dissipation rates and residues of fungicide azoxystrobin in ginseng and soil at two different cultivated regions in China.

    PubMed

    Hou, Zhiguang; Wang, Xiumei; Zhao, Xiaofeng; Wang, Xinhong; Yuan, Xing; Lu, Zhongbin

    2016-07-01

    The maximum residue limit (MRL) for fungicide azoxystrobin in ginseng has not yet been established in China. This is partially due to the lack of its dissipation and residue data at China's main ginseng production areas. In this work, the dissipation rates and residue levels of azoxystrobin in ginseng roots, plant parts (stems and leaves), and soil in Beijing and Jilin Province, China were determined using gas chromatograph-mass spectrometry (GC-MS). The mean half-life of azoxystrobin in ginseng plant parts was 1.6 days with a dissipation rate of 90 % over 21 days. The mean half-life in soil was 2.8 days with a dissipation rate of 90 % over 30 days. Dissipation rates from two geographically separated experimental fields differed, suggesting that these were affected by local soil characteristics and climate. Maximum final residues of azoxystrobin in ginseng roots, plant parts, and soil were determined to be 0.343, 9.40, and 0.726 mg kg(-1), respectively. Our results, particularly the high residues of azoxystrobin observed in ginseng plant parts, provide a quantitative basis for revising the application of this pesticide to ginseng.

  14. Development of an enzyme immunoassay for the antibiotic cefquinome and its application for residue determination in cow's milk after therapeutical mastitis treatment.

    PubMed

    Thal, Johannes; Steffen, Monika; Meier, Bianca; Schneider, Elisabeth; Adriany, Ansgar; Usleber, Ewald

    2011-01-01

    The aim of this study was to develop and evaluate an enzyme immunoassay (EIA) for the cephalosporin antibiotic in milk, in combination with a new microbiological test system (brilliant black reduction test, BRT-P). Polyclonal antibodies against cefquinome were produced in rabbits, using cefquinome-keyhole limpet hemocyanine as the immunogen. These antibodies and a cefquinome-glucose oxidase conjugate were used in a competitive indirect EIA. The detection limit for cefquinome in milk was 1.5 ng ml(-1), recoveries were 80-128% at 4-40 ng ml(-1). Cross-reactivities with other cephalosporins/penicillins were all <1%. The EIA was used to determine cefquinome in incurred raw milk, the BRT-P (detection limit ≈ 20 ng ml(-1)) and a receptor assay (ßeta-s.t.a.r., detection limit ≈ 15 ng ml(-1)) were used in parallel. Five lactating cows, suffering from clinical mastitis, were treated with cefquinome by simultaneous intramammary and intramuscular injection. Cefquinome residues (maximum 10-27 μg ml(-1)) were most exclusively found in the udder quarter which was treated intramammary, residue levels in the other three quarters were low (<20 ng ml(-1)). Even in milk from intramammary-dosed quarters, residue levels fell below European Union maximum residue level (MRL, 20 μg kg(-1)) 2 days before the end of the withdrawal period. EIA, BRT-P, and ßeta-s.t.a.r. results showed acceptable agreement for milk samples, but the newly developed EIA is superior in aspects of sensitivity. In conclusion, this is the first one description of immunoassay and microbiological tests capable to determine cefquinome in milk at the MRL in incurred sample material.

  15. Evaluation of the Presence and Levels of Enrofloxacin, Ciprofloxacin, Sulfaquinoxaline and Oxytetracycline in Broiler Chickens after Drug Administration

    PubMed Central

    da Silva, Guilherme Resende; Lanza, Isabela Pereira; Ribeiro, Ana Cláudia dos Santos Rossi; Lana, Ângela Maria Quintão; Lara, Leonardo José Camargos

    2016-01-01

    The depletion times of enrofloxacin and its metabolite ciprofloxacin as well as sulfaquinoxaline and oxytetracycline were evaluated in broiler chickens that had been subjected to pharmacological treatment. The presence and residue levels of these drugs in muscle tissue were evaluated using an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method that was validated in this work. The results showed the presence of all antimicrobial residues; however, the presence of residues at concentrations higher than the drugs’ maximum residue limit (MRL) of 100 μg kg-1 was found only during the treatment period for oxytetracycline and until two days after discontinuation of the medication for enrofloxacin, ciprofloxacin and sulfaquinoxaline. It was concluded that the residues of all antimicrobials were rapidly metabolized from the broiler muscles; after four days of withdrawal, the levels were lower than the limit of quantification (LOQ) of the method for the studied analytes. PMID:27846314

  16. Evaluation of the Presence and Levels of Enrofloxacin, Ciprofloxacin, Sulfaquinoxaline and Oxytetracycline in Broiler Chickens after Drug Administration.

    PubMed

    de Assis, Débora Cristina Sampaio; da Silva, Guilherme Resende; Lanza, Isabela Pereira; Ribeiro, Ana Cláudia Dos Santos Rossi; Lana, Ângela Maria Quintão; Lara, Leonardo José Camargos; de Figueiredo, Tadeu Chaves; Cançado, Silvana de Vasconcelos

    2016-01-01

    The depletion times of enrofloxacin and its metabolite ciprofloxacin as well as sulfaquinoxaline and oxytetracycline were evaluated in broiler chickens that had been subjected to pharmacological treatment. The presence and residue levels of these drugs in muscle tissue were evaluated using an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method that was validated in this work. The results showed the presence of all antimicrobial residues; however, the presence of residues at concentrations higher than the drugs' maximum residue limit (MRL) of 100 μg kg-1 was found only during the treatment period for oxytetracycline and until two days after discontinuation of the medication for enrofloxacin, ciprofloxacin and sulfaquinoxaline. It was concluded that the residues of all antimicrobials were rapidly metabolized from the broiler muscles; after four days of withdrawal, the levels were lower than the limit of quantification (LOQ) of the method for the studied analytes.

  17. Detection limits of antimicrobials in ewe milk by delvotest photometric measurements.

    PubMed

    Althaus, R L; Torres, A; Montero, A; Balasch, S; Molina, M P

    2003-02-01

    The Delvotest method detection limits per manufacturer's instructions at a fixed reading time of 3 h for 24 antimicrobial agents were determined in ewe milk by photometric measurement. For each drug, eight concentrations were tested on 20 ewe milk samples from individual ewes. Detection limits, determined by means of logistic regression models, were (microg/kg): 3, amoxycillin; 2, ampicillin; 18, cloxacillin; 1, penicillin "G"; 34, cefadroxil; 430, cephalosporin "C"; 40, cephalexin; 20, cefoperazone; 33, Ceftiofur; 18, cefuroxime; 6100, streptomycin; 1200, gentamycin; 2600, neomycin; 830, erythromycin; 100, tylosin; 180, doxycycline; 320, oxytetracycline; 590, tetracycline; 88, sulfadiazine; 44, sulfamethoxazole; 140, sulfametoxypyridazine; 48, sulfaquinoxaline; 12,000, chloramphenicol; and 290, trimethoprim. Whereas the beta-lactam antibiotics, sulphonamides, and tylosin were detected by Delvotest method at levels equal to those of maximum residue limits, its sensitivity needs to be enhanced to detect aminoglycosides, tetracyclines, streptomycin, chloramphenicol, and trimethoprim residues in ewe milk or to develop an integrated residue detection system for ewe milk with different sensitive microorganisms for each group of antiinfectious agents.

  18. Monitoring of pesticide residues of five notable vegetables at Agbogbloshie market in Accra, Ghana.

    PubMed

    Osei-Fosu, P; Donkor, A K; Nyarko, S; Nazzah, N K; Asante, I K; Kingsford-Adabo, R; Arkorful, N A

    2014-11-01

    The study monitored the concentrations of pesticide residues in vegetables arriving at Agbogbloshie, a central market in the Accra Metropolis from different parts of Ghana and beyond. A total of 810 samples of 5 different vegetables from Central, Volta, Greater Accra, Ashanti, Eastern Regions, and neighboring country (Togo) were collected from January 2009 through to December 2011. In all, 18 % of the samples had no detectable residues, 62 % were below the maximum residue limits (MRLs), and 20 % also exceeded the EU (MRLs) adopted values. Overall, lettuce contained the highest number of residues above their MRLs besides cucumber and cabbage. The pesticide residues were mainly organophosphates and synthetic pyrethroids. The results demonstrate the need for continuous monitoring of pesticide residues in vegetables arriving at the various major markets in Ghana.

  19. 76 FR 36349 - Diethylene Glycol MonoEthyl Ether (DEGEE); Exemption From the Requirement of a Tolerance

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-06-22

    ... use on growing crops and raw agricultural commodities, without limitation. Huntsman, Dow AgroSciences... a maximum permissible level for residues of DEGEE on growing crops and raw agricultural commodities... antifreeze [[Page 36350

  20. Degradation kinetics and safety evaluation of buprofezin residues in grape (Vitis vinifera L.) and three different soils of India.

    PubMed

    Oulkar, Dasharath P; Banerjee, Kaushik; Patil, Sangram H; Upadhyay, Ajay K; Taware, Praveen B; Deshmukh, Madhukar B; Adsule, Pandurang G

    2009-02-01

    This work was undertaken to determine the preharvest interval (PHI) of buprofezin to minimize its residues in grapes and thereby ensure consumer safety and avoid possible non-compliance in terms of residue violations in export markets. Furthermore, the residue dynamics in three grapevine soils of India was explored to assess its environmental safety. Residues dissipated following non-linear two-compartment first + first-order kinetics. In grapes, the PHI was 31 days at both treatments (312.5 and 625 g a.i. ha(-1)), with the residues below the maximum permissible intake even 1 h after foliar spraying. Random sampling of 5 kg comprising small bunchlets (8-10 berries) collected from a 1 ha area gave satisfactory homogeneity and representation of the population. A survey on the samples harvested after the PHI from supervised vineyards that received treatment at the recommended dose showed residues below the maximum residue limit (MRL) of 0.02 mg kg(-1) applicable for the European Union. In soil, the degradation rate was fastest in clay soil, followed by sandy loam and silty clay, with a half-life within 16 days in all the soils. The recommendation of the PHI proved to be effective in minimizing buprofezin residues in grapes. Thus, this work is of high practical significance to the domestic and export grape industry of India to ensure safety compliance in respect of buprofezin residues, keeping in view the requirements of international trade.

  1. Experimental Investigation of Principal Residual Stress and Fatigue Performance for Turned Nickel-Based Superalloy Inconel 718.

    PubMed

    Hua, Yang; Liu, Zhanqiang

    2018-05-24

    Residual stresses of turned Inconel 718 surface along its axial and circumferential directions affect the fatigue performance of machined components. However, it has not been clear that the axial and circumferential directions are the principle residual stress direction. The direction of the maximum principal residual stress is crucial for the machined component service life. The present work aims to focuses on determining the direction and magnitude of principal residual stress and investigating its influence on fatigue performance of turned Inconel 718. The turning experimental results show that the principal residual stress magnitude is much higher than surface residual stress. In addition, both the principal residual stress and surface residual stress increase significantly as the feed rate increases. The fatigue test results show that the direction of the maximum principal residual stress increased by 7.4%, while the fatigue life decreased by 39.4%. The maximum principal residual stress magnitude diminished by 17.9%, whereas the fatigue life increased by 83.6%. The maximum principal residual stress has a preponderant influence on fatigue performance as compared to the surface residual stress. The maximum principal residual stress can be considered as a prime indicator for evaluation of the residual stress influence on fatigue performance of turned Inconel 718.

  2. Captan and fenitrothion dissipation in field-treated cauliflowers and effect of household processing.

    PubMed

    Fernández-Cruz, María L; Barreda, Mercedes; Villarroya, Mercedes; Peruga, Arantzazu; Llanos, Susana; García-Baudín, José M

    2006-07-01

    Field trial studies have been performed with captan and fenitrothion on cauliflower to propose maximum residue limits and to study the dissipation of the pesticides. Residue levels have been determined at different times following good laboratory practice using gas chromatography with mass spectrometric detection. The behaviour of residue levels of these compounds after household processing has been analysed using gas chromatography with electron capture detection. Seven days after treatment, residue levels of captan could be detected, but not of fenitrothion. The half-lives of dissipation for captan and fenitrothion were calculated as 0.9 and 1.8 days respectively. Washing did not significantly affect the residual amounts of captan and fenitrothion observed in raw vegetables; however, after cooking, captan had degraded completely, whereas residue levels of fenitrothion were not modified significantly.

  3. Acephate and buprofezin residues in olives and olive oil.

    PubMed

    Cabras, P; Angioni, A; Garau, V L; Pirisi, F M; Cabitza, F; Pala, M

    2000-10-01

    Field trials were carried out to study the persistence of acephate and buprofezin on olives. Two cultivars, pizz'e carroga and pendolino, with very large and small fruits respectively were used. After treatment, no difference was found between the two pesticide deposits on the olives. The disappearance rates, calculated as pseudo first order kinetics, were similar for both pesticides (on average 12 days). Methamidophos, the acephate metabolite, was always present on all olives, and in some pendolino samples it showed higher residues than the maximum residue limit (MRL). During washing, the first step of olive processing, the residue level of both pesticides on the olives did not decrease. After processing of the olives into oil, no residues of acephate or methamidophos were found in the olive oil, while the residues of buprofezin were on average four times higher than on olives.

  4. Pesticide residues in raspberries (Rubus idaeus L.) and dietary risk assessment.

    PubMed

    Łozowicka, B; Kaczyński, P; Jankowska, M; Rutkowska, E; Hrynko, I

    2012-01-01

    The aim of this study was to evaluate the residues of 140 pesticides in raspberries from north-eastern Poland (2005-2010). Gas chromatography with electron capture detector (GC-ECD) and nitrogen phosphorous detector (GC-NPD) was used. Among the 128 samples, 66 (51.6%) were found to detect residues: 14.1% contained one pesticide and around 38% multiple pesticide residues. The most frequently detected were pyrimethanil residues (36.0%). Twenty-seven (21.1%) raspberry samples exceeded the maximum residue limits. The estimated daily intakes ranged from 0.003% to 3.183% of the acceptable daily intake (ADI) for adults 0.008% and 9.7% for toddlers, respectively. The most critical case is procymidone, the acute risk was 180.9% of acute reference dose (ARfD) for toddlers and for adults (83% of ARfD) which is high.

  5. Pesticide Residues in Honey from the Major Honey Producing Forest Belts in Ghana.

    PubMed

    Darko, Godfred; Addai Tabi, Jonah; Adjaloo, Michael Kodwo; Borquaye, Lawrence Sheringham

    2017-01-01

    Concentrations of pesticides residues in honey sampled from the major honey producing forest belts in Ghana were determined. Samples were purposively collected and extracted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method and analysed for synthetic pyrethroids, organochlorine, and organophosphate pesticide residues. Aldrin, γ -HCH, β -HCH, ∑endosulfan, cyfluthrin, cypermethrin, deltamethrin, permethrin methoxychlor, ∑DDT, chlorpyrifos, fenvalerate, malathion, dimethoate, and diazinon were all detected at the concentration of 0.01 mg/kg, while cyfluthrin and permethrin were detected at mean concentrations of 0.02 and 0.04 mg/kg, respectively. All the pesticide residues detected were very low and below their respective maximum residue limits set by the European Union. Hence, pesticide residues in honey samples analyzed do not pose any health risk to consumers.

  6. Rate of degradation of lambda-cyhalothrin and methomyl in grapes (Vitis vinifera L.).

    PubMed

    Banerjee, Kaushik; Upadhyay, Ajay Kumar; Adsule, Pandurang G; Patil, Sangram H; Oulkar, Dasharath P; Jadhav, Deepak R

    2006-10-01

    Rates of degradation of lambda-cyhalothrin and methomyl residues in grape are reported. The dissipation behavior of both insecticides followed first-order rate kinetics with similar patterns at standard and double-dose applications. Residues of lambda-cyhalothrin were lost with pre-harvest intervals (PHI) of 12.0-12.5 and 15.0-15.5 days, corresponding to the applications at 25 and 50 g a.i. ha-1, respectively. In the case of methomyl, residues were lost with PHI of 55.0 and 61.0 days, following applications at 1 and 2 kg a.i. ha-1, respectively. The PHI, recommended on the basis of the experimental results, was shown to be effective in minimizing residue load of these insecticides below their maximum residue limits (MRLs) in vineyard samples.

  7. Antimicrobials in beekeeping.

    PubMed

    Reybroeck, Wim; Daeseleire, Els; De Brabander, Hubert F; Herman, Lieve

    2012-07-06

    The bee diseases American and European foulbrood and nosemosis can be treated with anti-infectious agents. However, in the EU and the USA the use of these agents in beekeeping is strictly regulated due to the lack of tolerance (e.g. Maximum Residue Limit) for residues of antibiotics and chemotherapeutics in honey. This article reviews the literature dealing with antimicrobials of interest in apiculture, stability of these antimicrobials in honey, and disposition of the antimicrobials in honeybee hives. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. 77 FR 48899 - Flutriafol; Pesticide Tolerances for Emergency Exemptions

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-08-15

    ... cotton, undelinted seed; cotton, meal; cotton, refined oil; and cotton gin byproducts. This action is in..., and Rodenticide Act (FIFRA) authorizing use of the pesticide on cotton. This regulation establishes a maximum permissible level for residues of flutriafol in or on cotton commodities. The time-limited...

  9. The disappearance rate and risk assessment of thiacloprid residues in Asian pear using liquid chromatography confirmed with tandem mass spectrometry.

    PubMed

    Kabir, Md Humayun; Abd El-Aty, A M; Rahman, Md Musfiqur; Kim, Sung-Woo; Choi, Jeong-Heui; Lee, Young-Jun; Truong, Lieu T B; Lee, Kang-Bong; Kim, Mi-Ra; Shin, Ho-Chul; Shim, Jae-Han

    2017-05-01

    This study was undertaken to quantify the residue levels and propose the dissipation kinetics of thiacloprid formulated as suspension concentrate in field-incurred Asian pears grown under two different open-field conditions. Samples were extracted with 20% distilled water in acetonitrile; partitioned with brine water and dichloromethane; and purified with a Florisil solid phase extraction cartridge. The analyte was identified with an LC ultraviolet detector, and field-incurred samples were confirmed using LC-MS/MS. The calibration curve was linear over the range 0.05-5.0 mg/L with a satisfactory coefficient of determination (R 2  = 0.9994). The limits of detection and limits of quantification (LOQ) were 0.003 and 0.01 mg/kg, respectively. The recovery rate fortified to blank samples at LOQ, 10× LOQ, and the maximum residue limit (MRL) were between 73.7 and 86.2% with relative standard deviation ≤9.0%. The residual concentrations at both sites were considerably lower than the MRL (0.7 mg/kg) set by the Korean Ministry of Food Drug Safety, with biological half-lives of 5.0 and 7.4 days, for sites 1 and 2, respectively. From the pre-harvest residue limit curve, it was predicted that if the residues were <1.13 or 1.40 mg/kg 10 days before harvest, the residue level would be lower than the MRL during harvest. Risk assessment on day 0 showed an acceptable daily intake (%) of 13.0% and 11.0% for sites 1 and site 2, respectively, which indicates that the residual amounts are not hazardous to the Korean population. Copyright © 2016 John Wiley & Sons, Ltd.

  10. Identification of multi-insecticide residues using GC-NPD and the degradation kinetics of chlorpyrifos in sweet corn and soils.

    PubMed

    Wang, Peidan; Rashid, Muhammad; Liu, Jie; Hu, Meiying; Zhong, Guohua

    2016-12-01

    Because more than one insecticide is applied to crops to protect plants from pests, an analytical multi-residue determination method was developed using gas chromatography with a nitrogen phosphorus detector (GC-NPD). The retention time for 12 insecticides was 3.7-27.7min. Under the selected conditions, the limits of detection (LOD) and quantification (LOQ) were below the maximum residue limits (MRLs) and in the range of 0.00315-0.05μgmL(-1) and 0.01-0.165μgmL(-1), respectively. Using GC-NPD, we investigated the dissipation dynamics and final residual levels of chlorpyrifos in sweet corn and soil and determined that the half-lives was 4-7days, that is, that chlorpyrifos is safe to use on sweet corn with a pre-harvest interval of 16-22days before harvest. These results provide new insights into chlorpyrifos degradation in plants and its environmental behavior. Copyright © 2016. Published by Elsevier Ltd.

  11. An Overview on Recent Progress in Electrochemical Biosensors for Antimicrobial Drug Residues in Animal-Derived Food

    PubMed Central

    Majdinasab, Marjan; Yaqub, Mustansara; Rahim, Abdur; Catanante, Gaelle; Hayat, Akhtar; Marty, Jean Louis

    2017-01-01

    Anti-microbial drugs are widely employed for the treatment and cure of diseases in animals, promotion of animal growth, and feed efficiency. However, the scientific literature has indicated the possible presence of antimicrobial drug residues in animal-derived food, making it one of the key public concerns for food safety. Therefore, it is highly desirable to design fast and accurate methodologies to monitor antimicrobial drug residues in animal-derived food. Legislation is in place in many countries to ensure antimicrobial drug residue quantities are less than the maximum residue limits (MRL) defined on the basis of food safety. In this context, the recent years have witnessed a special interest in the field of electrochemical biosensors for food safety, based on their unique analytical features. This review article is focused on the recent progress in the domain of electrochemical biosensors to monitor antimicrobial drug residues in animal-derived food. PMID:28837093

  12. Assessment of Dithiocarbamate Residues on Tomatoes Conventionally Grown in Uganda and the Effect of Simple Washing to Reduce Exposure Risk to Consumers.

    PubMed

    Atuhaire, Aggrey; Kaye, Emmanuel; Mutambuze, Innocent Louis; Matthews, Graham; Friedrich, Theodor; Jørs, Erik

    2017-01-01

    Pesticide misuse by farmers poses health risks to consumers. This study assessed the level of dithiocarbamate residues in tomatoes acquired from 20 farmers and 25 market vendors in Wakiso District, how simple washing affects these residues, and the potential chronic health risk for Ugandans eating such tomatoes. Results revealed that mancozeb was the only reported dithiocarbamate, and 47.4% and 14% of farm and market samples, respectively, had dithiocarbamate residues exceeding the Codex alimentarius maximum residue limit of 2 mgCS 2 /kg. Mixing concentration had a positive significant effect on dithiocarbamate residue levels ( P = 0.004). Washing reduced dithiocarbamate residues by a factor of 0.3. Dietary risk assessment revealed no chronic health risk to both children and general population when a national daily per capita consumption of 1.0 g is considered. This study recommends comprehensive research into Uganda's food production and consumption patterns and establishment of a national pesticide residue surveillance program.

  13. Assessment of Dithiocarbamate Residues on Tomatoes Conventionally Grown in Uganda and the Effect of Simple Washing to Reduce Exposure Risk to Consumers

    PubMed Central

    Atuhaire, Aggrey; Kaye, Emmanuel; Mutambuze, Innocent Louis; Matthews, Graham; Friedrich, Theodor; Jørs, Erik

    2017-01-01

    Pesticide misuse by farmers poses health risks to consumers. This study assessed the level of dithiocarbamate residues in tomatoes acquired from 20 farmers and 25 market vendors in Wakiso District, how simple washing affects these residues, and the potential chronic health risk for Ugandans eating such tomatoes. Results revealed that mancozeb was the only reported dithiocarbamate, and 47.4% and 14% of farm and market samples, respectively, had dithiocarbamate residues exceeding the Codex alimentarius maximum residue limit of 2 mgCS2/kg. Mixing concentration had a positive significant effect on dithiocarbamate residue levels (P = 0.004). Washing reduced dithiocarbamate residues by a factor of 0.3. Dietary risk assessment revealed no chronic health risk to both children and general population when a national daily per capita consumption of 1.0 g is considered. This study recommends comprehensive research into Uganda’s food production and consumption patterns and establishment of a national pesticide residue surveillance program. PMID:28615952

  14. Cross-Sectional And Longitudinal Uncertainty Propagation In Drinking Water Risk Assessment

    NASA Astrophysics Data System (ADS)

    Tesfamichael, A. A.; Jagath, K. J.

    2004-12-01

    Pesticide residues in drinking water can vary significantly from day to day. However, drinking water quality monitoring performed under the Safe Drinking Water Act (SDWA) at most community water systems (CWSs) is typically limited to four data points per year over a few years. Due to limited sampling, likely maximum residues may be underestimated in risk assessment. In this work, a statistical methodology is proposed to study the cross-sectional and longitudinal uncertainties in observed samples and their propagated effect in risk estimates. The methodology will be demonstrated using data from 16 CWSs across the US that have three independent databases of atrazine residue to estimate the uncertainty of risk in infants and children. The results showed that in 85% of the CWSs, chronic risks predicted with the proposed approach may be two- to four-folds higher than that predicted with the current approach, while intermediate risks may be two- to three-folds higher in 50% of the CWSs. In 12% of the CWSs, however, the proposed methodology showed a lower intermediate risk. A closed-form solution of propagated uncertainty will be developed to calculate the number of years (seasons) of water quality data and sampling frequency needed to reduce the uncertainty in risk estimates. In general, this methodology provided good insight into the importance of addressing uncertainty of observed water quality data and the need to predict likely maximum residues in risk assessment by considering propagation of uncertainties.

  15. Residue depletion of tilmicosin in cattle after subcutaneous administration.

    PubMed

    Jiang, Haiyang; Ding, Shuangyang; Li, Jiancheng; An, Dianjin; Li, Cun; Shen, Jianzhong

    2006-07-12

    A study of tissue residue depletion of tilmicosin in cattle was conducted after a single subcutaneous injection at the therapeutic level of 10 mg per kg body weight. Eighteen cross cattle were treated with the tilmicosin oil formulation (30%). Three treated animals (two males and one female) were selected randomly to be scarified at 1, 7, 14, 28, and 35 days withdrawal after injection. Samples of the injection site and of muscle, liver, kidney, and fat were collected. Tilmicosin residue concentrations were determined using a high-performance liquid chromatography (HPLC) method with a UV detector at 290 nm. Using a statistical method recommended by the Committee for Veterinary Medical Products of European Medical Evaluation Agency, the withdrawal time of 34 days was established when all tissue residues except samples in the injection site were below the accepted maximum residue limits.

  16. Fate of vinclozolin, thiabendazole and dimethomorph during storage, handling and forcing of chicory.

    PubMed

    Spanoghe, Pieter; Ryckaert, Bert; Van Gheluwe, Cindy; Van Labeke, Marie-Christine

    2010-02-01

    As part of ongoing research for a sustainable production of Belgian endives, the fate of three fungicides during storage, handling and forcing of witloof chicory roots was investigated. Storage roots are protected against Sclerotinia sp. Fuckel and Phoma exigua var. exigua Desm. by means of vinclozolin and thiabendazole respectively. During hydroponic forcing, the most imminent pathogen is Phytophthora cryptogea Pethybr. & Laff., which is controlled by the use of dimethomorph. Vinclozolin and thiabendazole concentrations on roots remained constant during storage at -1 degrees C. Dermal exposure of the workers in hydroponics was exceeded. Vinclozolin and thiabendazole residues were not detected 2 weeks after hydroponic forcing; dimethomorph was still detected at harvest. At harvest, the vinclozolin concentration in the chicory heads was below the maximum residue limit, but the chicory roots contained residues much above the thiabendazole and dimethomorph maximum residue level. Vinclozolin and thiabendazole residues applied before storage are still present on the roots at the start of the forcing cycle. During the set-up of chicory roots, preventive measures are recommended, as effects of repeated human exposure to low doses of applied fungicides cannot be excluded. Dimethomorph applied at the start of the hydroponic forcing is the only pesticide detected in the drainage water at harvest. The chicory heads were safe for human consumption. However, more attention should be paid to the residues of fungicides in the roots used for cattle feeding.

  17. Bioefficacy, dissipation kinetics and safety evaluation of selected insecticides in Allium cepa L.

    PubMed

    Srinivas P, Satya; Banerjee, Kaushik; Jadhav, Manjusha R; Ghaste, Manoj S; Lawande, K E

    2012-01-01

    This paper reports the bioefficacy of selected insecticides against thrips and their pre-harvest intervals (PHI) in onion pertaining to their recommended application rates and maximum residue limits. Profenophos, methomyl and imidacloprid showed comparatively higher bioefficacy against thrips. GC-MS and LC-MS/MS-based residue analysis methods in onion bulbs and composite matrix of bulbs+leaves were thoroughly validated. The residue data for bulb+leaves was assessed with reference to the EU-MRLs applicable for spring onion. Dimethoate was the most stable chemical with PHI of 52.5 days, followed by monocrotophos (24 days) and carbofuran (20.5 days). The PHIs of profenophos, chlorpyrifos, methomyl and cypermethrin were similar and within the range of 10-13 days. Imidacloprid and λ-cyhalothrin had similar PHI of 4.5 days. Spinosad was the fastest-degrading chemical with PHI of 2 days. The combined bioefficacy and residue dynamics information will support label-claim of these insecticides for the management of thrips in onion, help in scheduling their applications in pest management program as per relative PHIs and minimize the residue accumulations at harvest. The dietary exposure was less than the maximum permissible intake for most of the insecticides on all sampling days except for dimethoate and monocrotophos.

  18. Analysis of beta-lactam antibiotics in incurred raw milk by rapid test methods and liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

    PubMed

    Riediker, S; Diserens, J M; Stadler, R H

    2001-09-01

    A recently developed confirmatory LC-MS method has been applied to the quantification of five major beta-lactam antibiotics in suspect raw bovine milk samples that gave a positive response with receptor-based (BetaStar) and rapid microbial inhibitory screen tests (Delvotest SP). In total, 18 presumptive positive raw milk samples were reanalyzed; 16 samples showed traces of antibiotic residues that could be identified and quantified by the LC-MS method, ranging from the limits of confirmation up to 38 microg/kg. Of the positive samples, only five (approximately 30%) were found to be violative of EU maximum residue limits. The most frequently detected antibiotic residues were cloxacillin and penicillin G, the former often in combination with amoxicillin or ampicillin. This study compares the results obtained by the three methods on identical samples and addresses how these relate to certain criteria such as sensitivity and selectivity. Furthermore, the limitations of the LC-MS method and the potential impact of the presence of frequently more than one residue in the same milk sample on the response of the rapid test methods are discussed.

  19. Solvent cleaning of pole transformers containing PCB contaminated insulating oil.

    PubMed

    Kanbe, H; Shibuya, M

    2001-01-01

    In 1989, it was discovered that the recycled insulation oil in pole transformers for electric power supply was contaminated with trace amounts of polychlorinated biphenyls (PCBs; maximum 50 mg-PCB/kg-insulation oil). In order to remove the PCBs from transformer components using n-hexane as a solvent, we investigated the relationship between progressive stages of dismantling and cleaning results. The results are summarized as follows: (1) Based on the cleaning test results, we made an estimate of the residual PCB amount on iron and copper components. By dismantling the test pole transformers into the "iron core and coil portion" and cleaning the components, we achieved a residual PCB amount that was below the limit of detection (0.05 mg-PCB/kg-material). To achieve a residual PCB amount below the limit of detection for the transformer paper component, it was necessary to cut the paper into pieces smaller than 5 mm. We were unable to achieve a residual PCB amount below the limit of detection for the wood component. (2) Compared to Japan's stipulated limited concentration standard values for PCBs, the results of the cleaning test show that cleaning iron or copper components with PCBs only on their surface with the solvent n-hexane will satisfy the limited concentration standard values when care is taken to ensure the component surfaces have adequate contact with the cleaning solvent.

  20. Chlorpyrifos residual behaviors in field crops and transfers during duck pellet feed processing.

    PubMed

    Li, Rui; Wei, Wei; He, Liang; Hao, Lili; Ji, Xiaofeng; Zhou, Yu; Wang, Qiang

    2014-10-22

    Chlorpyrifos is a widely used organophosphorus pesticide in agricultural crops (including food) and animal feeds in China, resulting in heavy contamination. Many studies have focused on the food-processing effects on chlorpyrifos removal, but sufficient information is not observed for feed-processing steps. Here, chlorpyrifos residual behaviors in field crops and its transfers in duck pellet feed-processing steps were evaluated. In field trials, the highest residues for rice grain, shelled corn, and soybean seed were 12.0, 0.605, and 0.220 mg/kg, respectively. Residues of all rice grain and about half of shelled corn exceeded the maximum residue limits (MRLs) of China, and five soybean seeds exceeded the MRL of China. Chlorpyrifos residue was reduced 38.2% in brown rice after the raw rice grain was hulled. The residue in bran increased 71.2% after milling from brown rice. During the squashing step, the residue reduced 73.8% in soybean meal. The residues reduced significantly (23.7-36.8%) during the process of granulating for rice, maize, and soybean products. Comparatively, the grinding process showed only limited influence on chlorpyrifos removal (<10%). The residues of duck pellet feeds produced from highly contaminated raw materials of this study were 1.01 mg/kg (maize-soybean feed) and 3.20 mg/kg (rice-soybean feed), which were much higher than the generally accepted value (>0.1 mg/kg) for animal feeding. Chlorpyrifos residues were removed significantly by processing steps of pellet feeds, but the residue of raw materials was the determining factor for the safety of duck feeding.

  1. Manufacture of reconstruction-bricks in Mexico

    NASA Astrophysics Data System (ADS)

    Rojas-Valencia, Ma. Neftalí; Penagos, Armando Aguilar; Rojas, Denise Y. Fernández; López, Alberto López; Gálves, David Morillón

    2017-12-01

    In Mexico, around 33.600 tons of construction wastes are generated every day, Mexico City contributing for around tons/day, with fewer than 1.000 tons/day being sent to be recycled. For that reason the purpose of this study was to manufacture sustainable bricks, based on three types of wastes generated in the building industry: wood cutting residues, wastes from the excavation process (From Coapa and Cuautlancingo, Puebla, Mexico) and recycled aggregates. Water was added as kneading material, and Opuntia ficus-indica (mucilage) was supplemented as natural additive to improve the workability of the mixtures. Conventional firing process was substituted by drying in a solar drying chamber. Nine mixtures were prepared using 62% excavation wastes, 4% wood cutting residues and 11%, 17% and 34% recycled aggregates. These mixtures were classified in two groups depending on their granulometry: the first one denominated cementitious recycled aggregates only having granulometry from 25.4 mm, 9.52 mm to 6.35 mm to fines and the second group denominated all in one recycled aggregates having granulometry of 6.35 mm to fines. The quality of the sustainable bricks was evaluated according to compressive strength and water absorption parameters. The results of nine mixtures showed that the reconstruction-bricks manufactured with the mixture seven consisting of 9.52 mm and 6.35 mm construction residues (all in one) fines presented the highest strength values, lowest maximum initial absorption (4 g/min) compared to the norm NMX-C-037-ONNCCE-2013 which establishes that the maximum limit for walls exposed to the outside is 5 g/min. Using a solar desiccator made from construction residues, the bricks were dried in 11 days, the maximum temperature was 76 °C and the maximum solar radiation captured was 733.4 W/m2.

  2. Validation of a liquid chromatography-electrospray ionization tandem mass spectrometric method to determine six polyether ionophores in raw, UHT, pasteurized and powdered milk.

    PubMed

    Pereira, Mararlene Ulberg; Spisso, Bernardete Ferraz; Jacob, Silvana do Couto; Monteiro, Mychelle Alves; Ferreira, Rosana Gomes; Carlos, Betânia de Souza; da Nóbrega, Armi Wanderley

    2016-04-01

    This study aimed to validate a method developed for the determination of six antibiotics from the polyether ionophore class (lasalocid, maduramicin, monensin, narasin, salinomycin and semduramicin) at residue levels in raw, UHT, pasteurized and powdered milk using QuEChERS extraction and high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The validation was conducted under an in-house laboratory protocol that is primarily based on 2002/657/EC Decision, but takes in account the variability of matrix sources. Overall recoveries between 93% and 113% with relative standard deviations up to 16% were obtained under intermediate precision conditions. CCα calculated values did not exceed 20% the Maximum Residue Limit for monensin and 25% the Maximum Levels for all other substances. The method showed to be simple, fast and suitable for verifying the compliance of raw and processed milk samples regarding the limits recommended by Codex Alimentarius and those adopted in European Community for polyether ionophores. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Residues of lambda-cyhalothrin in tea.

    PubMed

    Seenivasan, Subbiah; Muraleedharan, Narayanan Nair

    2009-02-01

    Field experiments were conducted at two places in Tamil Nadu (India) during dry season of 2006 to determine the residues of lambda-cyhalothrin in fresh green tea leaves and black tea. Residues were quantified at different harvest intervals of '0' (3h), 1st, 3rd, 5th, 7th, 10th and 14th day after insecticide application. Persistence, dissipation pattern, half-life value and safe harvest interval of the insecticide in tea were calculated. Residues of lambda-cyhalothrin dissipated exponentially after application at both the locations and reached below the European Union maximum residue limit (MRL) of 1mg/kg on the 5th day. Lambda-cyhalothrin showed that like other insecticides it followed the first order dissipation kinetics. Half-life values varied from 2.8 to 3.5 days for lambda-cyhalothrin and a safety harvest interval of 5 days is suggested for tea at the recommended dosage.

  4. Survey on the pesticide residues in tea in south India.

    PubMed

    Seenivasan, Subbiah; Muraleedharan, NarayananNair

    2011-05-01

    Tea is considered as a 'health beverage' due its antioxidant properties and resultant beneficial effects on human health. Such a beverage should be free from toxic elements such as pesticide residues and heavy metals. A large scale survey of teas produced in the tea factories of south India had been carried out for a period of three years from 2006 to 2008 and 912 tea samples were analysed for the residues of certain pesticides such as dicofol, ethion, quinalphos, hexaconazole, fenpropathrin, fenvalerate and propargite which are used for pest and disease control in tea in this part of the country. The analytical data proved that only less than 0.5 percentage of tea samples had residues of these pesticides. However, residues of pesticides were below their maximum limits in tea, stipulated by the European Union, Codex Alimentarius Commission of FAO/WHO and Prevention of Food Adulteration Act of Govt. of India.

  5. Behavior of myclobutanil, propiconazole, and nuarimol residues during lager beer brewing.

    PubMed

    Navarro, Simón; Pérez, Gabriel; Vela, Nuria; Mena, Luis; Navarro, Ginés

    2005-11-02

    Over a 4 month brewing process, the fate of three fungicides, myclobutanil, propiconazole, and nuarimol, was studied in the spent grain, brewer wort, and final beer product. Only the residual level of myclobutanil after the mashing step was higher than its maximum residue limit (MRL) on barley. A substantial fraction was removed with the spent grain in all cases (26-42%). The half-life times obtained for the fungicides during storage of the spent grains ranged from 82 to 187 days. No significant influence of the boiling stage on the decrease of the fungicide residues was demonstrated. During fermentation, the content reduction varied from 20 to 47%. After the lagering and filtration steps, no significant decrease (<10%) was observed in any of the residues. Finally, during storage of the beer (3 months), the amounts of fungicides fell by 25-50% of their respective concentrations in the finished beer.

  6. Determination of bromothalonil residues and degradation in apple and soil by QuEChERS and GC-MS/MS.

    PubMed

    Liu, Huijun; Guo, Baoyuan; Wang, Huili; Li, Jianzhong; Zheng, Lin

    2014-04-01

    The dissipation and residues of bromothalonil in apple and soil under field condition were analyzed by QuEChERS (quick, easy, cheap, effective, rugged and safe) combined with gas chromatography-mass spectrometer method. The recoveries were ranged from 80.8 % to 106 % with coefficient variation for repeatability ranged from 3.08 % to 7.09 % at fortification levels of 0.02, 0.04 and 0.2 mg/kg in apple and soil. The limit of quantification of the method was 0.31 μg/kg. The dissipation rates of bromothalonil followed the first-order kinetics and the half-lives were from 3.61 to 3.98 days in apple and from 4.65 to 9.29 days in soil. In apple, the terminal residues of bromothalonil were below the China maximum residue limit (0.2 mg/kg) after 7 days of application. This work contributed to provide the basic information for a safe usage of bromothalonil in apple orchard and preventing health problem from consumers in China.

  7. Dissipation, transfer and safety evaluation of emamectin benzoate in tea.

    PubMed

    Zhou, Li; Luo, Fengjian; Zhang, Xinzhong; Jiang, Yaping; Lou, Zhengyun; Chen, Zongmao

    2016-07-01

    The dissipation and residue of emamectin benzoate in tea leaves and the residue transfer from tea leaves to tea brew were investigated by modified QuEChERS (quick, easy, cheap, effective, rugged and safe) combined with ultra performance liquid chromatography tandem mass (UPLC-MS/MS). The average recoveries ranged 85.3-101.3% with relative standard deviation (RSD) less than 15%. The limits of quantification (LOQ) were 0.005mgkg(-1) in tea leaves and 0.0004mgL(-1) in brew. Emamectin benzoate dissipated rapidly in tea with half-life (t1/2) of 1.0-1.3days. The terminal residues of emamectin benzoate were less than 0.062mgkg(-1). The leaching rate of emamectin benzoate from freshly-made tea to brew was <5%. The risk of emamectin benzoate at the recommended dosage was negligible to humans depending on risk quotient (RQ) value, that was lower than 1 significantly. This study could provide guidance for the safe use of emamectin benzoate and serve as a reference for the establishment of maximum residue limits (MRLs) in China. Copyright © 2016. Published by Elsevier Ltd.

  8. Determination of critical levels of residual oxygen to minimize discoloration of sliced packaged Norwegian salami under light display.

    PubMed

    Sørheim, Oddvin; Måge, Ingrid; Larsen, Hanne

    2017-07-01

    Discoloration of sliced packaged salami is contributing to rejection of the product, food waste and economical loss. A combination of residual O 2 in the headspace of packages and light is causing photooxidation and deterioration of colour. The aim of this study was to establish maximum tolerable concentrations of residual O 2 in packages of salami slices with 100% N 2 under light display at 4 and 20°C. Salami sausages had variable inherent O 2 consumption rate. Storage of salami in 1% O 2 in darkness did not induce discoloration. The upper limits for O 2 for avoiding discoloration under light were variable in the range 0.1-1.0%, depending on temperature and type of salami. Display at 20°C increased the rate of O 2 depletion compared to 4°C. To minimize discoloration, sliced and packaged salami should be stored in darkness at approximately 20°C until the level of residual O 2 is reduced below a critical limit. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. High-throughput method for the determination of residues of β-lactam antibiotics in bovine milk by LC-MS/MS.

    PubMed

    Jank, Louise; Martins, Magda Targa; Arsand, Juliana Bazzan; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara

    2015-01-01

    This study describes the development and validation procedures for scope extension of a method for the determination of β-lactam antibiotic residues (ampicillin, amoxicillin, penicillin G, penicillin V, oxacillin, cloxacillin, dicloxacillin, nafcillin, ceftiofur, cefquinome, cefoperazone, cephapirine, cefalexin and cephalonium) in bovine milk. Sample preparation was performed by liquid-liquid extraction (LLE) followed by two clean-up steps, including low temperature purification (LTP) and a solid phase dispersion clean-up. Extracts were analysed using a liquid chromatography-electrospray-tandem mass spectrometry system (LC-ESI-MS/MS). Chromatographic separation was performed in a C18 column, using methanol and water (both with 0.1% of formic acid) as mobile phase. Method validation was performed according to the criteria of Commission Decision 2002/657/EC. Main validation parameters such as linearity, limit of detection, decision limit (CCα), detection capability (CCβ), accuracy, and repeatability were determined and were shown to be adequate. The method was applied to real samples (more than 250) and two milk samples had levels above maximum residues limits (MRLs) for cloxacillin - CLX and cefapirin - CFAP.

  10. Occurrence of antimicrobial residues in Brazilian food animals in 2008 and 2009.

    PubMed

    Nonaka, C K V; Oliveira, A M G; Paiva, C R; Almeida, M P; Rezende, C P; Moraes, C G O; Botelho, B G; Souza, L F; Dias, P G

    2012-01-01

    Brazil is one of the most important countries as a producer and exporter of cattle and poultry. In 2009 cattle accounted for 30% of the export market and 41.4% for poultry meat. The Brazilian National Residues and Contaminants Control Plan (PNCRC) follows the guidelines set by the Codex Alimentarius Commission and checks compliance maximum residue limits (MRLs) to ensure the quality of these commodities. Kidney samples (n = 2978) were analysed between January 2008 and December 2009. Fifteen antibiotics of the macrolide and aminoglycoside groups (clindamycin, eritromycin, lincomycin, tylmicosin, tylosin, amikacin, apramycin, dihydrostreptomycin, gentamycin, higromycin, kanamycin, neomycin, spectinomycin, streptomycin, tobramycin) were determined by a microbiological screening method (FAST) and confirmed/quantified using liquid chromatography (LC-MS/MS and UPLC-MS/MS). In 2008, 1459 samples were analysed by a screening test and liquid chromatography with only one sample (0.07%) exceeded Brazilian legislation limits (>MRL). In 2009, 1519 samples were analysed and none exceeding Brazilian legislation limits (>MRL). The slaughterhouses of 16 states were monitored during the year of 2008, and 18 states were monitored in 2009, being the major producing states most sampled by the PNCRC.

  11. Pesticides and their metabolites in wells of Suffolk County, New York, 1998

    USGS Publications Warehouse

    Phillips, Patrick J.; Eckhardt, D.A.; Terracciano, S.A.; Rosenmann, Larry

    1999-01-01

    Five insecticide residues and 20 herbicide residues were detected in water samples collected from 50 shallow wells screened in the surficial sand and gravel aquifer in Suffolk County, Long Island in areas with known or suspected residues. Laboratory analytical methods with extremely low detection limits - from 0.001 to 0.2 ?g/L (micrograms per liter) - were used to analyze the samples for 60 pesticide residues. Forty-four of the samples contained at least one pesticide residue, and some samples contained as many as 11 different pesticides or pesticide metabolites. Only four water- quality standards were exceeded in the samples collected in this study. Dieldrin exceeded the New York State Class GA standard (0.004 ?g/L) in samples from eight wells. The Federal and New York State Maximum Contaminant Level for simazine (4 ?g/L) was exceeded in samples from two wells, and the State Class GA standard for simazine (0.5 ?g/L) was exceeded in samples from six wells. Federal water-quality standards have not been established for many of the compounds detected in this study, including herbicide metabolites. Maximum concentrations of four herbicide metabolites -metolachlor ESA (ethanesulfonic acid), metolachlor OA (oxanilic acid), and the alachlor metabolites alachlor ESA and alachlor OA -exceeded 20 ?g/L. The maximum concentration of one herbicide (tebuthiuron) exceeded 10 ?g/L, and the maximum concentration of three herbicides (simazine, metolachlor, and atrazine) and one herbicide metabolite (deisopropylatrazine) ranged from 1 to 10 ?g/L. The herbicide metolachlor, which is used on potato fields in Suffolk County, and its metabolites (metolachlor ESA and metolachlor OA) were most frequently detected in samples from agricultural areas. The herbicides simazine and tebuthiuron, which were used in utility rights-of-way, and the simazine metabolite deisopropylatrazine were detected at concentrations greater than 0.05 ?g/L most frequently in samples from residential and mixed land-use areas. The results of this investigation are not necessarily representative of conditions throughout the remainder of Long Island, because these samples were collected in areas of known or suspected residues.

  12. Detection of β-Lactams and Chloramphenicol Residues in Raw Milk-Development and Application of an HPLC-DAD Method in Comparison with Microbial Inhibition Assays.

    PubMed

    Karageorgou, Eftychia; Christoforidou, Sofia; Ioannidou, Maria; Psomas, Evdoxios; Samouris, Georgios

    2018-06-01

    The present study was carried out to assess the detection sensitivity of four microbial inhibition assays (MIAs) in comparison with the results obtained by the High Performance Liquid Chromatography with Diode-Array Detection (HPLC-DAD) method for antibiotics of the β-lactam group and chloramphenicol in fortified raw milk samples. MIAs presented fairly good results when detecting β-lactams, whereas none were able to detect chloramphenicol at or above the permissible limits. HPLC analysis revealed high recoveries of examined compounds, whereas all detection limits observed were lower than their respective maximum residue limits (MRL) values. The extraction and clean-up procedure of antibiotics was performed by a modified matrix solid phase dispersion procedure using a mixture of Plexa by Agilent and QuEChERS as a sorbent. The HPLC method developed was validated, determining the accuracy, precision, linearity, decision limit, and detection capability. Both methods were used to monitor raw milk samples of several cows and sheep, obtained from producers in different regions of Greece, for the presence of examined antibiotic residues. Results obtained showed that MIAs could be used effectively and routinely to detect antibiotic residues in several milk types. However, in some cases, spoilage of milk samples revealed that the kits' sensitivity could be strongly affected, whereas this fact does not affect the effectiveness of HPLC-DAD analysis.

  13. Residue depletion of tilmicosin in chicken tissues.

    PubMed

    Zhang, Yue; Jiang, Haiyang; Jin, Xingjun; Shen, Zhangqi; Shen, Jianzhong; Fu, Caixia; Guo, Junlin

    2004-05-05

    A high-performance liquid chromatography (HPLC) method with detection at 290 nm was modified and validated for the determination of tilmicosin residues in broiler chicken tissues. The limits of detection (LOD) of the method were 0.01 microg/g for muscle and 0.025 microg/g for liver and kidney. Average recoveries ranged from 80.4 to 88.3%. Relative standard deviation values ranged from 5.2 to 12.1%. Residue depletion of tilmicosin in broiler chickens was examined after dosing over a 5-day period by incorporation of the drug into drinking water at 37.5 and 75.0 mg/L. Tilmicosin concentrations in liver and kidney were highest on day 3 of medication and on day 5 in muscle, in both low- and high-dose groups. The residue levels in both groups were significantly higher in liver than in kidney or muscle. A minimum withdrawal time of 9 days was indicated for residue levels in muscle, liver, and kidney tissues below the maximum residue level (MRL).

  14. Pesticide residues in orange fruit from citrus orchards in Nuevo Leon State, Mexico.

    PubMed

    Suárez-Jacobo, Angela; Alcantar-Rosales, Victor Manuel; Alonso-Segura, Diana; Heras-Ramírez, Maria; Elizarragaz-De La Rosa, Dalau; Lugo-Melchor, Ofelia; Gaspar-Ramirez, Octavio

    2017-09-01

    Some international organisations established maximum residue limits (MRLs) in food to protect human health. Mexico lacks regulations in this matter, affecting national and international trade from agroindustry. The aim of this study was to diagnose pesticide residues in oranges from Nuevo Leon, México, in citrus orchards. In May 2014, 100 orange fruit samples were taken randomly from orchards and subjected to analysis for 93 pesticides at residual level by GC/QQQ-MS and LCQ-TOF-MS. Results showed the presence of 15 pesticide residues in the samples. The comparison of the residual levels of pesticides found in orange samples among the MRLs allowed by USA, EU and Japanese regulations demonstrated that all samples were below MRLs issued by USA and Japan. Some orange samples were above MRLs issued by the EU. This provides a basis to establish strategies in order to satisfy International Standards to protect human health and encourage Food Safety in Mexico.

  15. Residues of organochlorine and synthetic pyrethroid pesticides in honey, an indicator of ambient environment, a pilot study.

    PubMed

    Malhat, Farag M; Haggag, Mohamed N; Loutfy, Naglaa M; Osman, Mohamed A M; Ahmed, Mohamed Tawfic

    2015-02-01

    Samples of honey were screened to monitor residues of organochlorine and pyrethroid pesticides. The study meant to examine the quality of honey, and to use honey as a bioindicator of environmental contamination. Residue levels were determined by gas chromatography (GC-μECD). Samples had a wide spectrum of organochlorine and synthetic pyrethroids pesticides, with hexachlorobenzene (HCB) as the most frequently detected organochlorine, followed by permethrin, heptachlor epoxide. Only one sample had a concentration of γ-HCH higher than maximum residue limit of honey (0.01 mg kg(-1)). Residues of organochlorines detected, indicate the presence of some fresh supplies, despite the ban imposed on their use. The study confirmed that honey bee and beehive matrices could be used as gauge for monitoring environment contamination. From public health point of view, the observed levels of pesticide residues in honey do not pose a serious health risk to the consumers, but raises questions of the source of organochlorines. Copyright © 2014 Elsevier Ltd. All rights reserved.

  16. Pyrethroids in chicken eggs from commercial farms and home production in Rio de Janeiro: Estimated daily intake and diastereomeric selectivity.

    PubMed

    Parente, Cláudio E T; Lestayo, Julliana; Guida, Yago S; Azevedo-Silva, Claudio E; Torres, João Paulo M; Meire, Rodrigo O; Malm, Olaf

    2017-10-01

    In this study, pyrethroids were determined in chicken eggs from commercial farm (n = 60) and home egg production (n = 30). These pyrethroids were investigated: bifenthrin, phenothrin, permethrin, cyfluthrin, cypermethrin and fenvalerate, including most diastereomers. Quantification was done using GC-MS in a negative chemical ionization mode. Pyrethroids residues were found in 79% of the analyzed samples. Cypermethrin presented the highest occurrence, being quantified in 62 samples (69%) in concentrations (lipid weight - l w.) varying between 0.29 and 6408 ng g -1 , followed by phenothrin (24%), 21-3910 ng g -1 , permethrin (14%), 2.96-328 ng g -1 , and bifenthrin (11%), 3.77-16.7 ng g -1 . Cyfluthrin and fenvalerate were not detected. Home-produced eggs had a higher occurrence of pyrethroids (97%), with a greater predominance of phenothrin. In commercial production, 70% of the samples presented pyrethroid residues (predominantly cypermethrin). This is the first report about the presence of pyrethroids in home-produced eggs and the first description of a selectivity pattern with the predominance of cis diastereomers in chicken eggs. In general, estimated daily intake does not present a risk to human consumption, according to Brazilian and international standards (FAO/WHO). However, one third of the samples (30 eggs) had concentrations above the maximum residue limits (MRLs). The maximum cypermethrin concentration was 66 times the MRL, while the maximum phenothrin concentration was 11 times the limit. Further studies about transfer dynamics, bioaccumulation and metabolic degradation of stereoisomers are required, as well as determining if this selectivity pattern in food can increase consumer's health risk. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Disappearance of six pesticides in fresh and processed zucchini, bioavailability and health risk assessment.

    PubMed

    Oliva, J; Cermeño, S; Cámara, M A; Martínez, G; Barba, A

    2017-08-15

    A field study was carried out on the dissipation of three insecticides and three fungicides during the freezing of zucchini. A simultaneous residue analysis method is validated using QuEChERS extraction with acetonitrile and CG-MS and LC-MS analysis. The residues detected after field application never exceeded the established maximum residue limits. The processing factors calculated (fresh product/frozen product) are lower than 1, indicating a clear influence of the stages of the freezing process, especially the washing and blanching. The in vitro study of bioavailability establishes a low percentage of stomach absorption capacity. The level of residues detected in fresh zucchini and the Estimated Daily Intake calculated for Spain suggest that there is no risk of acute toxicity due to dietary exposure. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. Doxycycline and sulfadimethoxine transfer from cross-contaminated feed to chicken tissues.

    PubMed

    Segato, G; Benetti, C; Angeletti, R; Montesissa, C; Biancotto, G

    2011-01-01

    During feed preparation at feed mills or during feed mixing in bins at farms, the accidental contamination of feed at trace levels by veterinary drug residues, commonly known as carry-over, can accidentally but frequently occur. To evaluate the concentrations of residual antimicrobials in poultry edible tissues, due to contaminated feed, sulfadimethoxine and doxycycline were administered for 10 days to chickens in poultry feed incurred at the contamination levels frequently found during national feed monitoring programmes (1-5 mg kg(-1)). Sulfadimethoxine and doxycycline residual concentrations detected in muscle (

  19. Expression and characterization of a new esterase with GCSAG motif from a permafrost metagenomic library.

    PubMed

    Petrovskaya, Lada E; Novototskaya-Vlasova, Ksenia A; Spirina, Elena V; Durdenko, Ekaterina V; Lomakina, Galina Yu; Zavialova, Maria G; Nikolaev, Evgeny N; Rivkina, Elizaveta M

    2016-05-01

    As a result of construction and screening of a metagenomic library prepared from a permafrost-derived microcosm, we have isolated a novel gene coding for a putative lipolytic enzyme that belongs to the hormone-sensitive lipase family. It encodes a polypeptide of 343 amino acid residues whose amino acid sequence displays maximum likelihood with uncharacterized proteins from Sphingomonas species. A putative catalytic serine residue of PMGL2 resides in a new variant of a recently discovered GTSAG sequence in which a Thr residue is replaced by a Cys residue (GCSAG). The recombinant PMGL2 was produced in Escherichia coli cells and purified by Ni-affinity chromatography. The resulting protein preferably utilizes short-chain p-nitrophenyl esters (C4 and C8) and therefore is an esterase. It possesses maximum activity at 45°C in slightly alkaline conditions and has limited thermostability at higher temperatures. Activity of PMGL2 is stimulated in the presence of 0.25-1.5 M NaCl indicating the good salt tolerance of the new enzyme. Mass spectrometric analysis demonstrated that N-terminal methionine in PMGL2 is processed and cysteine residues do not form a disulfide bond. The results of the study demonstrate the significance of the permafrost environment as a unique genetic reservoir and its potential for metagenomic exploration. © FEMS 2016. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  20. A New Load Residual Threshold Definition for the Evaluation of Wind Tunnel Strain-Gage Balance Data

    NASA Technical Reports Server (NTRS)

    Ulbrich, N.; Volden, T.

    2016-01-01

    A new definition of a threshold for the detection of load residual outliers of wind tunnel strain-gage balance data was developed. The new threshold is defined as the product between the inverse of the absolute value of the primary gage sensitivity and an empirical limit of the electrical outputs of a strain{gage. The empirical limit of the outputs is either 2.5 microV/V for balance calibration or check load residuals. A reduced limit of 0.5 microV/V is recommended for the evaluation of differences between repeat load points because, by design, the calculation of these differences removes errors in the residuals that are associated with the regression analysis of the data itself. The definition of the new threshold and different methods for the determination of the primary gage sensitivity are discussed. In addition, calibration data of a six-component force balance and a five-component semi-span balance are used to illustrate the application of the proposed new threshold definition to different types of strain{gage balances. During the discussion of the force balance example it is also explained how the estimated maximum expected output of a balance gage can be used to better understand results of the application of the new threshold definition.

  1. 77 FR 8741 - Spirotetramat; Pesticide Tolerances for Emergency Exemptions

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-02-15

    ... on onion, dry bulb under section 408(l)(6) of the Federal Food, Drug, and Cosmetic Act (FFDCA), 21 U... pesticide on dry bulb onions. This regulation establishes a maximum permissible level for residues of... degradates, in or on onion, dry bulb at 0.3 parts per million (ppm). This time-limited tolerance expires on...

  2. Determination of tylosin residues in pig tissues using high-performance liquid chromatography.

    PubMed

    De Liguoro, M; Anfossi, P; Angeletti, R; Montesissa, C

    1998-06-01

    In accordance with the maximum residue limit of 100 micrograms kg-1 established by EU legislation, a simple and sensitive high-performance liquid chromatographic (HPLC) method was developed for the measurement of tylosin residues in pig tissues (fat, kidney, liver and muscle). Tylosin, a macrolide antibiotic, is extracted with water-methanol and cleaned-up by solid-phase extraction (SPE) on cation-exchange cartridges using methanol elution. Tylosin was determined by reversed-phase HPLC with UV detection at 280 nm and the mean recovery from pig tissues fortified in the range 50-200 micrograms kg-1 was 70-85%, with intra- and inter-day RSDs in the ranges 3.4-9.1 and 3.9-10.1% respectively.

  3. Dissipation pattern and risk assessment studies of triazophos residues on capsicum (Capsicum annuum L.) using GLC-FPD and GC-MS.

    PubMed

    Singh, Yadwinder; Mandal, Kousik; Singh, Balwinder

    2015-10-01

    The present study was carried out to observe the dissipation pattern of triazophos on capsicum and risk assessment of its residues on human beings and to suggest a waiting period for the safety of consumers. Following two applications of triazophos (Truzo 40 EC) at 500 and 1000 g a.i. ha(-1), the average initial deposits were found to be 3.61 and 6.26 mg kg(-1), respectively. These residues dissipated below the limit of quantification (LOQ) of 0.05 mg kg(-1) in 10 and 15 days at the recommended and double the recommended dosages, respectively. The calculated values of half-life were 2.31 and 2.14 days at recommended and double the recommended dosages, respectively. Theoretical maximum residue contribution (TMRC) values were found to be 28.8 and 41.6 μg person(-1) day(-1) at 500 and 1000 g a.i. ha(-1), respectively, and found to be below the maximum permissible intake on capsicum fruit on the 7th day. Therefore, a waiting period of 7 days is suggested for consumption of capsicum sprayed with triazophos at the recommended dosages.

  4. Determination of cyflumetofen residue in water, soil, and fruits by modified quick, easy, cheap, effective, rugged, and safe method coupled to gas chromatography/tandem mass spectrometry.

    PubMed

    Li, Minmin; Liu, Xingang; Dong, Fengshou; Xu, Jun; Qin, Dongmei; Zheng, Yongquan

    2012-10-01

    A new, highly sensitive, and selective method was developed for the determination of the cyflumetofen residue in water, soil, and fruits by using gas chromatography quadruple mass spectrometry. The target compound was extracted using acetonitrile and then cleaned up using dispersive solid-phase extraction with primary and secondary amine and graphitized carbon black, and optionally by a freezing-out cleanup step. The matrix-matched standards gave satisfactory recoveries and relative standard deviation values in different matrices at three fortified levels (0.05, 0.5, and 1.0 mg kg(-1) ). The overall average recoveries for this method in water, soil, and all fruits matrix at three fortified levels ranged from 76.3 to 101.5% with relative standard deviations in the range of 1.2-11.8% (n = 5). The calculated limits of detection and quantification were typically below 0.005 and 0.015 μg kg(-1), which were much lower than the maximum residue levels established by Japanese Positive List. This study provides a theoretical basis for China to draw up maximum residue level and analytical method for cyflumetofen acaricide in different fruits. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Dissipation dynamic, residue distribution and processing factor of hexythiazox in strawberry fruits under open field condition.

    PubMed

    Saber, Ayman N; Malhat, Farag M; Badawy, Hany M A; Barakat, Dalia A

    2016-04-01

    Two independent field trials were performed to investigate the dissipation and residue levels of hexythiazox in strawberry. The study presents a method validation for extraction and quantitative analysis of hexythiazox residues in strawberry using HPLC-DAD. The results shown that the mean recoveries ranged from 85% to 93%, furthermore the intra- and inter-day relative standard deviations were less than 10%. The results suggest that the hexythiazox dissipation curves followed the first-order kinetic and its half-life ranged from 3.43 to 3.81 days. The final residues in strawberry were below the Codex maximum residue limit (MRL) (6 mg/kg) after three days of the application. The effects of household processing and storage on the levels of hexythiazox residues were quantified, and it's useful for reducing the dietary exposure. The processing factor after each stage were generally less than 1, indicating that the whole process can reduce the residues of hexythiazox in strawberry. The results could provide guidance to safe and reasonable use of hexythiazox in agriculture. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. Determination of lasalocid residues in the tissues of broiler chickens by liquid chromatography-tandem mass spectrometry.

    PubMed

    Tkáčiková, Soňa; Kožárová, Ivona; Mačanga, Ján; Levkut, Martin

    2012-01-01

    Lasalocid is a polyether ionophoric coccidiostat used for the prevention of coccidiosis in poultry at a prescribed concentration and during a certain time interval. Due to a public health concern about the presence of coccidiostat residues in poultry, the aim of the present study was to determine the levels of lasalocid residues in the edible tissues of broiler chickens (breast muscle, thigh muscle, heart, liver, gizzard, kidneys and skin/fat) fed commercially produced feed containing 100 mg kg⁻¹) of lasalocid in complete feed throughout the 5-day withdrawal period (WP). The residues were investigated by liquid chromatography coupled with electrospray ionisation (ESI) tandem mass spectrometry (MS/MS) with triple quadrupole. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 0.47 and 1.44 µg kg⁻¹, respectively. The average recovery based on the matrix-fortified calibrations for chicken tissues ranged between 79% and 98%. Lasalocid was found to accumulate in the liver, followed by the heart, skin/fat, kidneys, thigh muscle and gizzard. The lowest concentrations of lasalocid residues were found in the breast muscle. On day 5 of the WP, residue concentrations of lasalocid did not decline below the LOQ of the method, but were far below the maximum residue level (MRL) established for lasalocid in poultry from 20 to 100 µg kg⁻¹ by European Commission Regulation (EU) No. 37/2010. The results confirmed that the WP established for lasalocid is sufficient to ensure the decline of its residues in the tissues of broiler chickens to the safe residue level.

  7. Monitoring of streptomycin and dihydrostreptomycin residual levels in porcine meat press juice and muscle via solid-phase fluorescence immunoassay and confirmatory analysis by liquid chromatography after post-column derivatization.

    PubMed

    Pyun, Chang-Won; Abd El-Aty, A M; Hashim, M M M; Shim, Jae-Han; Lee, Si-Kyung; Choi, Kang-Duk; Park, Kwan-Ha; Shin, Ho-Chul; Lee, Chiho

    2008-03-01

    A solid-phase fluorescence immunoassay (SPFIA) that was primarily developed for detection of antibiotic residues in milk was qualitatively applied for the pre-screening of the residues of aminoglycoside antibiotics, streptomycin and dihydrostreptomycin, in meat press juice. The confirmation of both analytes was performed using a validated method of highperformance liquid chromatography with post-column derivatization. The analytical performance was demonstrated by the analysis of pork meat samples spiked at three concentration levels, ranging from 0.25 to 2.5 ppm for each analyte. In general, the recoveries ranged from 80.4 to 81.5% and from 79.6 to 84.4% for streptomycin and dihydrostreptomycin, respectively, with relative standard deviations lower than 6%. The limits of detection were 0.1 and 0.15 ppm for streptomycin and dihydrostreptomycin, respectively, and the limits of quantification of 0.35 and 0.5 ppm are below the maximum residue limits of Codex, the European Union, and the Korean Food and Drug Administration (ranging from 0.5 to 0.6 ppm). Eight real samples collected from the Seoul area were first monitored using SPFIA, and none of them were found positive. These findings are in good accordance with those observed by HPLC analysis. To the best of our knowledge, this is the first report to monitor the aminoglycoside residues in pork meat press juice using SPFIA.

  8. Dissipation and residue of azoxystrobin in banana under field condition.

    PubMed

    Wang, Siwei; Sun, Haibin; Liu, Yanping

    2013-09-01

    A method was developed for determining azoxystrobin in banana and cultivation soil using gas chromatography. The dissipation and residue of azoxystrobin in banana fields at GAP conditions were investigated. The average recoveries ranged from 80.3 to 96.0 % with relative standard deviations of 2.9 to 7.2 % at three different spiking levels for each matrix. The results indicated that the half-life of azoxystrobin in bananas and soil ranged from 7.5 to 13.5 days in Guangdong and from 8.7 to 12.7 days in Fujian. The dissipation rates of azoxystrobin in banana and soil were almost the same. Terminal residues in banana and banana flesh (0.01 mg/kg) were all below the maximum residue limit (2 mg/kg by Codex Alimentarius Commission and China). The results demonstrated that the safety of using azoxystrobin at the recommended agriculture dosage to protect bananas from diseases.

  9. 40 CFR 141.54 - Maximum residual disinfectant level goals for disinfectants.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... for disinfectants. MRDLGs for disinfectants are as follows: Disinfectant residual MRDLG(mg/L) Chlorine... 40 Protection of Environment 23 2014-07-01 2014-07-01 false Maximum residual disinfectant level goals for disinfectants. 141.54 Section 141.54 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY...

  10. 40 CFR 141.54 - Maximum residual disinfectant level goals for disinfectants.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... for disinfectants. MRDLGs for disinfectants are as follows: Disinfectant residual MRDLG(mg/L) Chlorine... 40 Protection of Environment 24 2012-07-01 2012-07-01 false Maximum residual disinfectant level goals for disinfectants. 141.54 Section 141.54 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY...

  11. 40 CFR 141.54 - Maximum residual disinfectant level goals for disinfectants.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... for disinfectants. MRDLGs for disinfectants are as follows: Disinfectant residual MRDLG(mg/L) Chlorine... 40 Protection of Environment 24 2013-07-01 2013-07-01 false Maximum residual disinfectant level goals for disinfectants. 141.54 Section 141.54 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY...

  12. 40 CFR 423.15 - New source performance standards (NSPS).

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... exceed (mg/l) TSS 100.0 30.0 Oil and grease 20.0 15.0 Copper, total 1.0 1.0 Iron, total 1.0 1.0 (e... pollutants from fly ash transport water. (h)(1) For any plant with a total rated electric generating capacity... or pollutant property NSPS effluent limitations Maximum concentration (mg/l) Total residual chlorine...

  13. A framework for streamflow prediction in the world's most severely data-limited regions: Test of applicability and performance in a poorly-gauged region of China

    NASA Astrophysics Data System (ADS)

    Alipour, M. H.; Kibler, Kelly M.

    2018-02-01

    A framework methodology is proposed for streamflow prediction in poorly-gauged rivers located within large-scale regions of sparse hydrometeorologic observation. A multi-criteria model evaluation is developed to select models that balance runoff efficiency with selection of accurate parameter values. Sparse observed data are supplemented by uncertain or low-resolution information, incorporated as 'soft' data, to estimate parameter values a priori. Model performance is tested in two catchments within a data-poor region of southwestern China, and results are compared to models selected using alternative calibration methods. While all models perform consistently with respect to runoff efficiency (NSE range of 0.67-0.78), models selected using the proposed multi-objective method may incorporate more representative parameter values than those selected by traditional calibration. Notably, parameter values estimated by the proposed method resonate with direct estimates of catchment subsurface storage capacity (parameter residuals of 20 and 61 mm for maximum soil moisture capacity (Cmax), and 0.91 and 0.48 for soil moisture distribution shape factor (B); where a parameter residual is equal to the centroid of a soft parameter value minus the calibrated parameter value). A model more traditionally calibrated to observed data only (single-objective model) estimates a much lower soil moisture capacity (residuals of Cmax = 475 and 518 mm and B = 1.24 and 0.7). A constrained single-objective model also underestimates maximum soil moisture capacity relative to a priori estimates (residuals of Cmax = 246 and 289 mm). The proposed method may allow managers to more confidently transfer calibrated models to ungauged catchments for streamflow predictions, even in the world's most data-limited regions.

  14. Residues and dissipation of kresoxim methyl in apple under field condition.

    PubMed

    Malhat, Farag; Kamel, Essam; Saber, Ayman; Hassan, Ehab; Youssef, Ahmed; Almaz, Monir; Hassan, Ayman; Fayz, Abd El-Salam

    2013-09-01

    The dissipation and residual levels of kresoxim methyl in apple under field condition were determined by using HPLC-DAD with QuEChERS method. At fortification levels of 0.05, 0.1, 0.5 and 1.0 mg kg(-1) in apple, it was shown that recoveries were ranged from 91.1% to 96.9% with coefficient variation of the method (CV%) for repeatability ranged from 1.27% to 4.77%. The limit of quantification (LOQ) of the method was 0.05 mg kg(-1). The dissipation rates of kresoxim methyl were described by using first-order kinetics and its half-life, as they are ranged from 4.58 to 4.77 days in apple. The terminal residues of kresoxim methyl were below the FAO/WHO maximum residue limit (MRL, 0.2 mg kg(-1)) in apple when measured 14 days after the final application, which suggested that the use of this fungicide was safe for humans. This study would help in providing the basic information for developing regulation to guard a safe use of kresoxim methyl in apple orchard and to prevent health problem from consumers. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Pesticide Residues in Commercial Lettuce, Onion, and Potato Samples From Bolivia-A Threat to Public Health?

    PubMed

    Skovgaard, Marlene; Encinas, Susana Renjel; Jensen, Olaf Chresten; Andersen, Jens Hinge; Condarco, Guido; Jørs, Erik

    2017-01-01

    Bolivia does not have a surveillance program for pesticide residues in food. The few published studies have suggested that pesticide contamination in food may present a public health problem. Data are lacking for all foods except tomatoes and breast milk. In this study 10 potato, 10 onion, and 10 lettuce samples from La Paz were sampled on August 15, 2015 at a local market and screened for 283 pesticides. Residues of cypermethrin, chlorpyrifos, difenoconazol, or/and λ-cyhalothrin were detected in 50% of the lettuce samples, whereas no pesticides were found in potatoes and onions. In 20% of the lettuce samples, the measurements were above the maximum residue limits, and 2 or 3 pesticides were identified simultaneously. Washing almost halved the pesticide levels, but still 20% of the samples showed measurements above the limits. No samples contained concentrations of pesticides which alone or together would lead to exposures that exceeded the acceptable daily intake or the acute reference dose. To protect consumers from pesticide poisonings and chronic effects, the development of measures for prevention, control, and monitoring of food contamination by pesticides in Bolivia is suggested.

  16. Pesticide Residues in Commercial Lettuce, Onion, and Potato Samples From Bolivia—A Threat to Public Health?

    PubMed Central

    Skovgaard, Marlene; Renjel Encinas, Susana; Jensen, Olaf Chresten; Andersen, Jens Hinge; Condarco, Guido; Jørs, Erik

    2017-01-01

    Bolivia does not have a surveillance program for pesticide residues in food. The few published studies have suggested that pesticide contamination in food may present a public health problem. Data are lacking for all foods except tomatoes and breast milk. In this study 10 potato, 10 onion, and 10 lettuce samples from La Paz were sampled on August 15, 2015 at a local market and screened for 283 pesticides. Residues of cypermethrin, chlorpyrifos, difenoconazol, or/and λ-cyhalothrin were detected in 50% of the lettuce samples, whereas no pesticides were found in potatoes and onions. In 20% of the lettuce samples, the measurements were above the maximum residue limits, and 2 or 3 pesticides were identified simultaneously. Washing almost halved the pesticide levels, but still 20% of the samples showed measurements above the limits. No samples contained concentrations of pesticides which alone or together would lead to exposures that exceeded the acceptable daily intake or the acute reference dose. To protect consumers from pesticide poisonings and chronic effects, the development of measures for prevention, control, and monitoring of food contamination by pesticides in Bolivia is suggested. PMID:28469451

  17. Determination of 10 sulfonamide residues in meat samples by liquid chromatography with ultraviolet detection.

    PubMed

    Di Sabatino, Marcello; Di Pietra, Anna Maria; Benfenati, Luigi; Di Simone, Bruno

    2007-01-01

    A liquid chromatography (LC) method is described for the simultaneous determination of 10 commonly used sulfonamide drug residues in meat. The 10 sulfonamide drugs of interest were sulfadiazine, sulfathiazole, sulfamerazine, sulfadimidine, sulfamethizole, sulfamonomethoxine, sulfachloropyridazine, sulfadoxine, sulfadimethoxine, and sulfaquinoxaline. The residues were extracted with acetone-chloroform (1 + 1). Sulfonamides were quantitatively retained in the extracting solution and afterwards eluted from a cation-exchanger solid-phase extraction cartridge with a solution of methanol-aqueous ammonia. The solution was dried, reconstituted with 5 mL methanol and filtered before analysis by LC-ultraviolet using a C18 column with a mobile phase gradient of potassium dihydrogen phosphate buffer, pH 2.5, and methanol-acetonitrile (30 + 70, v/v). The method was applied to cattle, swine, chicken, and sheep muscle tissues. The validation was performed with a fortified cattle meat sample at level of 100 ppb, which is the administrative maximum residue limit for sulfonamides in the European Union. The limit of quantitation for all sulfonamides was between 3 and 14 ppb. Recovery was evaluated for different meat matrixes. The mean recovery values were between 66.3% for pork meat samples and 71.5% for cattle meat samples.

  18. Organochlorine and organophosphorus pesticide residues in fodder and milk samples along Musi river belt, India.

    PubMed

    Kotinagu, Korrapati; Krishnaiah, Nelapati

    2015-04-01

    The present study was conducted to find the organochlorine pesticide (OCP) and organophosphorus pesticide (OPP) residues in fodder and milk samples along Musi river belt, India. Fodder and milk samples collected from the six zones of Musi river belt, Hyderabad India were analyzed by gas chromatography with electron capture detector for OCP residues and pulsated flame photometric detector for the presence of OPP residues. The gas chromatographic analysis of fodder samples of Zone 5 of Musi river showed the residues of dicofol at concentration of 0.07±0.0007 (0.071-0.077). Among organophosphorus compounds, dimetheoate was present in milk samples collected from Zone 6 at a level of 0.13±0.006 (0.111-0.167). The residues of OCPs, OPPs and cyclodies were below the detection limit in the remaining fodder and milk samples collected from Musi river belt in the present study. The results indicate that the pesticide residues in fodder and milk samples were well below the maximum residue level (MRL) values, whereas dicofol in fodder and dimethoate in milk were slightly above the MRL values specified by EU and CODEX.

  19. Organochlorine and organophosphorus pesticide residues in fodder and milk samples along Musi river belt, India

    PubMed Central

    Kotinagu, Korrapati; Krishnaiah, Nelapati

    2015-01-01

    Aim: The present study was conducted to find the organochlorine pesticide (OCP) and organophosphorus pesticide (OPP) residues in fodder and milk samples along Musi river belt, India. Materials and Methods: Fodder and milk samples collected from the six zones of Musi river belt, Hyderabad India were analyzed by gas chromatography with electron capture detector for OCP residues and pulsated flame photometric detector for the presence of OPP residues. Results: The gas chromatographic analysis of fodder samples of Zone 5 of Musi river showed the residues of dicofol at concentration of 0.07±0.0007 (0.071-0.077). Among organophosphorus compounds, dimetheoate was present in milk samples collected from Zone 6 at a level of 0.13±0.006 (0.111-0.167). The residues of OCPs, OPPs and cyclodies were below the detection limit in the remaining fodder and milk samples collected from Musi river belt in the present study. Conclusion: The results indicate that the pesticide residues in fodder and milk samples were well below the maximum residue level (MRL) values, whereas dicofol in fodder and dimethoate in milk were slightly above the MRL values specified by EU and CODEX. PMID:27047132

  20. Evolution of titanium residue on the walls of a plasma-etching reactor and its effect on the polysilicon etching rate

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Hirota, Kosa, E-mail: hirota-kousa@sme.hitachi-hitec.com; Itabashi, Naoshi; Tanaka, Junichi

    2014-11-01

    The variation in polysilicon plasma etching rates caused by Ti residue on the reactor walls was investigated. The amount of Ti residue was measured using attenuated total reflection Fourier transform infrared spectroscopy with the HgCdTe (MCT) detector installed on the side of the reactor. As the amount of Ti residue increased, the number of fluorine radicals and the polysilicon etching rate increased. However, a maximum limit in the etching rate was observed. A mechanism of rate variation was proposed, whereby F radical consumption on the quartz reactor wall is suppressed by the Ti residue. The authors also investigated a plasma-cleaningmore » method for the removal of Ti residue without using a BCl{sub 3} gas, because the reaction products (e.g., boron oxide) on the reactor walls frequently cause contamination of the product wafers during etching. CH-assisted chlorine cleaning, which is a combination of CHF{sub 3} and Cl{sub 2} plasma treatment, was found to effectively remove Ti residue from the reactor walls. This result shows that CH radicals play an important role in deoxidizing and/or defluorinating Ti residue on the reactor walls.« less

  1. Multiclass method for the determination of 62 antibiotics in milk.

    PubMed

    Moretti, Simone; Cruciani, Gabriele; Romanelli, Sara; Rossi, Rosanna; Saluti, Giorgio; Galarini, Roberta

    2016-09-01

    A multiclass method for screening and confirmatory analysis of antimicrobial residues in milk has been developed and validated. Sixty-two antibiotics belonging to ten different drug families (amphenicols, cephalosporins, lincosamides, macrolides, penicillin, pleuromutilins, quinolones, rifamycins, sulfonamides and tetracyclines) have been included. After the addition of an aqueous solution of EDTA, the milk samples were extracted twice with acetonitrile, evaporated and dissolved in ammonium acetate. After centrifugation, 10 µl were analysed using LC-Q-Orbitrap operating in positive electrospray ionization mode. The method was validated in bovine milk in the range 2-150 µg kg(-1) for all antibiotics; for four compounds with maximum residue limits higher than 100 µg kg(-1) , the validation interval has been extended until 333 µg kg(-1) . The estimated performance characteristics were satisfactory complying with the requirements of Commission Decision 2002/657/EC. Good accuracies were obtained also taking advantage from the versatility of the hybrid mass analyser. Identification criteria were achieved verifying the mass accuracy and ion ratio of two ions, including the pseudomolecular one, where possible. Finally, the developed procedure was applied to 13 real cases of suspect milk samples (microbiological assay) confirming the presence of one or more antibiotics, although frequently, the maximum residue limits were not exceeded. The availability of rapid multiclass confirmatory methods can avoid wastes of suspect, but compliant, raw milk samples. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  2. The detection limits of antimicrobial agents in cow's milk by a simple Yoghurt Culture Test.

    PubMed

    Mohsenzadeh, M; Bahrainipour, A

    2008-09-15

    The aim of this study was to study performance of Yoghurt Culture Test (YCT) in the detection of antimicrobial residues in milk. For this purpose, the sensitivity of YCT for 15 antibiotics were determined. For each drug, 8 concentrations were tested. The detection limits of YCT at 2.5 h and 4 h incubation were determined (microg kg(-1)): 15 and 37.5, penicillin G; 4 and 5, ampicillin; 5 and 7.5, amoxycillin; 100 and 200, cephalexin; 80 and 100, cefazoline; 100 and 200, oxytetracycline; 500 and 100, chlortetracycline; 100 and 200, tetracycline; 150 and 200, doxycycline; 200 and 400, sulphadimidine; 500 and 1000, gentamycin; 1000 and 1500, spectinomycin; 400 and 500, erythromycin; 50 and 100, tylosin; 5000 and 10000, chloramphenicol. The YCT detection limits at 2.5 h incubation for ampicillin, cephalexin, tetracycline, oxytetracycline and tylosin are similar to those obtained as Maximum Residue Limit (MRL) according to Regulation 2377/90 EEC as set out by the European Union. In addition the detection limits of YCT for some antibiotics were lower than some of microbial inhibitor test.

  3. Validation of an UHPLC-MS/MS Method for Screening of Antimicrobial Residues in Eggs and Their Application to Analyses of Eggs from Laying Hens Subjected to Pharmacological Treatment

    PubMed Central

    Caldeira, Letícia Gomes Magnago; Santos, Flávio Alves; de Oliveira, Andréa Melo Garcia; Lima, Josefa Abucater; de Souza, Leonardo Francisco; da Silva, Guilherme Resende; de Assis, Débora Cristina Sampaio

    2017-01-01

    A multiresidue method by UHPLC/MS-MS was optimized and validated for the screening and semiquantitative detection of antimicrobials residues from tetracyclines, aminoglycosides, quinolones, lincosamides, β-lactams, sulfonamides, and macrolides families in eggs. A qualitative approach was used to ensure adequate sensitivity to detect residues at the level of interest, defined as maximum residue limit (MRL), or less. The applicability of the methods was assessed by analyzing egg samples from hens that had been subjected to pharmacological treatment with neomycin, enrofloxacin, lincomycin, oxytetracycline, and doxycycline during five days and after discontinuation of medication (10 days). The method was adequate for screening all studied analytes in eggs, since the performance parameters ensured a false-compliant rate below or equal to 5%, except for flumequine. In the analyses of eggs from laying hens subjected to pharmacological treatment, all antimicrobial residues were detected throughout the experimental period, even after discontinuation of medication, except for neomycin, demonstrating the applicability of the method for analyses of antimicrobial residues in eggs. PMID:29181222

  4. Degradation of chlorpyrifos residues in apple under temperate conditions of Kashmir Valley.

    PubMed

    Mukhtar, Malik; Sherwani, Asma; Wani, Ashraf Alam; Ahmed, Sheikh Bilal; Sofi, Javid Ahmad; Bano, Parveena

    2015-08-01

    The present studies were carried out to observe the dissipation pattern of chlorpyrifos on apple in Kashmir Valley. Persistence of chlorpyrifos in apple was studied following two applications rates of chlorpyrifos (Dursban 20 EC) at 200 g a.i. ha(-1) (single dose T 1) and 400 g a.i. ha(-1) (double dose T 2). The average initial deposit of chlorpyrifos was found to be 1.61 and 1.98 μg g(-1) for T 1 and T 2 application rates respectively on apple. The residues dissipated to 0.09 and 0.06 μg g(-1) after 15- and 30-day post treatment with half-life periods of 3.34 and 5.47 days in T 1 and T 2 application rates, respectively. The residues of chlorpyrifos dissipated to below limit of quantification (LOQ) of 0.04 μg g(-1) after 30 day at T 1 application rate. A waiting period of 6 days must be observed for chlorpyrifos on apple at recommended application rate for the safety of consumers. Theoretical maximum residue contribution (TMRC) values were found to be far less than maximum permissible intake (MPI) at 0 day in both the dosages suggesting chlorpyrifos on apple in Kashmir is unlikely to cause health risks.

  5. Organochlorine pesticide residues in ground water of Thiruvallur district, India.

    PubMed

    Jayashree, R; Vasudevan, N

    2007-05-01

    Modern agriculture practices reveal an increase in use of pesticides and fertilizers to meet the food demand of increasing population which results in contamination of the environment. In India crop production increased to 100% but the cropping area has increased marginally by 20%. Pesticides have played a major role in achieving the maximum crop production, but maximum usage and accumulation of pesticide residues was highly detrimental to aquatic and other ecosystem. The present study was chosen to know the level of organochlorines contamination in ground water of Thiruvallur district, Tamil Nadu, India. The samples were highly contaminated with DDT, HCH, endosulfan and their derivatives. Among the HCH derivatives, Gamma HCH residues was found maximum of 9.8 microg/l in Arumbakkam open wells. Concentrations of pp-DDT and op-DDT were 14.3 microg/l and 0.8 microg/l. The maximum residue (15.9 microg/l) of endosulfan sulfate was recorded in Kandigai village bore well. The study showed that the ground water samples were highly contaminated with organochlorine residues.

  6. Matrix-Matching as an Improvement Strategy for the Detection of Pesticide Residues.

    PubMed

    Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie

    2016-05-01

    More than 90% of the pesticides residues in apples are located in the peel. We developed a gas chromatography/ion trap tandem mass spectrometry method for investigating all detectable residues in the peel of 3 apple varieties. Sample preparation is based on the use of the Quick Easy Cheap Effective Rugged and Safe method on the whole fruit, the flesh, and the peel. Pesticide residues were quantified with solvent-matched and matrix-matched standards, by spiking apple sample extracts. Matrix effects dependent on the type of extract (fruit, flesh, or peel) and the apple variety were detected. The best data processing methods involved normalizing matrix effect rates by matrix-matched internal/external calibration. Boscalid, captan, chlorpyrifos, fludioxonil, and pyraclostrobin were the most frequently detected pesticides. However, their concentrations in the whole fruit were below European maximum residue levels. Despite negative matrix effects, the residues in peel were detected at concentrations up to 10 times higher than those in whole fruits. Consequently, other pesticide residues present at concentrations below the limit of quantification in the whole fruit were detected in the peel. © 2016 Institute of Food Technologists®

  7. Production of monoclonal antibody to acaricide dicofol and its derivatives.

    PubMed

    Hongsibsong, Surat; Prapamontol, Tippawan; Suphavilai, Chaisuree; Wipasa, Jiraprapa; Pattarawarapan, Mookda; Kasinrerk, Watchara

    2010-12-01

    In Thailand detection of acaricide dicofol residues has been sporadically performed due to the limitation of analytical techniques. Conventional analytical methods for detecting dicofol residues most often use chromatographic-based techniques. Our ultimate aim is to develop an alternative method for rapidly analyzing dicofol residues in vegetables and fruit samples. Here we report the production of monoclonal antibodies specific to dicofol and its derivatives. Hapten-protein carriers were prepared by linking succinic anhydride to dichlorobenzhydrol (DCBH), which was then conjugated to bovine serum albumin (BSA) and oval albumin (OVA). DCBH-BSA conjugate was used as immunogen while DCBH-OVA conjugate was used as capture antigen for competitive inhibition assay. Female BALB/c mice were immunized with DCBH-BSA conjugate subcutaneously, and antibody (Ab) level was determined 2 weeks after the last immunization. Spleen cells producing high titer antibody were isolated and fused with myeloma cells of P3.X6.Ag8.653. After limiting dilutions, antibody produced by one clone had high affinity, which was found to be of IgG1 with κ light chain. Specificity and inhibition concentrations of the monoclonal antibody (MAb) were determined by competitive indirect ELISA with dicofol, and its 50% (IC(50)) was 0.28 μg/mL. Working ranges of the developed immunoassay were from 0.07 to 25 μg/mL. Hence, the prepared MAb will be able to be applied for immunoassay development for detecting dicofol residue in vegetables and fruits far below the maximum residue limit such that 5 g of fruits and berries can be detected below 0.1 mg/kg.

  8. Validation of a method for the determination of 120 pesticide residues in apples and cucumbers by LC-MS/MS.

    PubMed

    Ramadan, Gouda; Al Jabir, Muna; Alabdulmalik, Najat; Mohammed, Ali

    2016-05-01

    Most countries have clearly defined regulations governing the use of pesticides in agricultural activity. The application of pesticides in agriculture usually leads to a residual amount of these pesticides on food products such as fruit and vegetables. The presence of pesticide residues on these foods destined for human consumption may pose food safety risks to consumers. To protect consumers, national authorities have established maximum limits for pesticide residues in foods. These limits can only be enforced if there are methods available to detect and monitor their concentrations in the applicable food products. To support the enforcement of this legislation, we have developed a multi-residue liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of 120 pesticide residues in apples and cucumbers which has been validated and implemented in the routine monitoring and surveillance programme for these pesticides. In this method, apple and cucumber samples are extracted using the QuEChERS method (quick, easy, cheap, effective, rugged, and safe) and the extracts were analyzed directly by LC-MS/MS. The mean recoveries at three different concentrations of 0.01 µg/g , 0.05 µg/g, and 0.1 µg/g over the analytical range varied between 70 and 120%. The repeatability of the method expressed as %RSD was less than 20%. The limit of detection (LOD) of the method ranged between 0.0014 and 0.0110 µg/g for apples and between 0.0012 and 0.0075 µg/g for cucumbers. The limit of quantification (LOQ) of the method was 0.01 µg/g for apples and cucumbers. The method has been used for the analysis of over 600 apple and 550 cucumber samples over the past two years. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  9. Dissipation rate study and pre-harvest intervals calculation of imidacloprid and oxamyl in exported Egyptian green beans and chili peppers after pestigation treatment.

    PubMed

    Hanafi, Ahmad; Dasenaki, Marilena; Bletsou, Anna; Thomaidis, Nikolaos S

    2018-02-01

    Two QuEChERS-based methods were developed and validated, using liquid chromatography-tandem mass spectrometric detection, in order to accurately determine residues of imidacloprid and oxamyl in green beans and chili peppers after treatment via irrigation system under field conditions in Egyptian farms. The validation included experiments for specificity, linearity, trueness, precision, matrix effect and limits of detection and quantification according to European Commission standards. The dissipation rates of both pesticides in green beans and chili peppers were studied and the pre-harvest intervals (PHIs) were calculated. The LOQ values of imidacloprid were 0.47 and 2.6μg/kg in green beans and chili peppers, respectively, while for oxamyl the LOQs were 2.9 and 0.67μg/kg, respectively. No PHI of imidacloprid is required, while for oxamyl it was found that still after 21days, its residues' concentration on both crops was significantly higher than the maximum residue limit. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Application of a luminescent bacterial biosensor for the detection of tetracyclines in routine analysis of poultry muscle samples.

    PubMed

    Pikkemaat, M G; Rapallini, M L B A; Karp, M T; Elferink, J W A

    2010-08-01

    Tetracyclines are extensively used in veterinary medicine. For the detection of tetracycline residues in animal products, a broad array of methods is available. Luminescent bacterial biosensors represent an attractive inexpensive, simple and fast method for screening large numbers of samples. A previously developed cell-biosensor method was subjected to an evaluation study using over 300 routine poultry samples and the results were compared with a microbial inhibition test. The cell-biosensor assay yielded many more suspect samples, 10.2% versus 2% with the inhibition test, which all could be confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Only one sample contained a concentration above the maximum residue limit (MRL) of 100 microg kg(-1), while residue levels in most of the suspect samples were very low (<10 microg kg(-1)). The method appeared to be specific and robust. Using an experimental set-up comprising the analysis of a series of three sample dilutions allowed an appropriate cut-off for confirmatory analysis, limiting the number of samples and requiring further analysis to a minimum.

  11. Fabric phase sorptive extraction of selected penicillin antibiotic residues from intact milk followed by high performance liquid chromatography with diode array detection.

    PubMed

    Samanidou, Victoria; Michaelidou, Katia; Kabir, Abuzar; Furton, Kenneth G

    2017-06-01

    Fabric phase sorptive extraction (FPSE), a novel sorbent-based microextraction method, was evaluated as a simple and rapid strategy for the extraction of four penicillin antibiotic residues (benzylpenicillin, cloxacillin, dicloxacillin and oxacillin) from cows' milk, without prior protein precipitation. Time-consuming solvent evaporation and reconstitution steps were eliminated successfully from the sample preparation workflow. FPSE utilizes a flexible fabric substrate, chemically coated with sol-gel derived, highly efficient, organic-inorganic hybrid sorbent as the extraction medium. Herein short-chain poly(ethylene glycol) provided optimum extraction sensitivity for the selected penicillins, which were analysed using an RP-HPLC method, validated according to the European Decision 657/2002/EC. The limit of quantitation was 10μg/kg for benzylpenicillin, 20μg/kg for cloxacillin, 25μg/kg dicloxacillin and 30μg/kg oxacillin. These are a similar order of magnitude with those reported in the literature and (with the exception of benzylpenicillin) are less than the maximum residue limits (MRL) set by European legislation. Copyright © 2016 Elsevier Ltd. All rights reserved.

  12. Analysis of abamectin residues in avocados by high-performance liquid chromatography with fluorescence detection.

    PubMed

    Hernández-Borges, Javier; Ravelo-Pérez, Lidia M; Hernández-Suárez, Estrella M; Carnero, Aurelio; Rodríguez-Delgado, Miguel Angel

    2007-09-21

    In this work an analytical method for the determination of abamectin residues in avocados is developed using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection. A pre-column derivatization with trifluoroacetic anhydride (TFAA) and N-methylimidazole (NMIM) was carried out. The mobile phase consisted of water, methanol and acetonitrile (5:47.5:47.5 v/v/v) and was pumped at a rate of 1 mL/min (isocratic elution). The fluorescence detector was set at an excitation wavelength of 365 nm and an emission wavelength of 470 nm. Homogenized avocado samples were extracted twice with acetonitrile:water 8:2 (v/v) and cleaned using C(18) solid-phase extraction (SPE) cartridges. Recovery values were in the range 87-98% with RSD values lower than 13%. The limits of detection (LODs) and quantification (LOQs) of the whole method were 0.001 and 0.003 mg/kg, respectively. These values are lower than the maximum residue limit (MRL) established by the European Union (EU) and the Spanish legislation in avocado samples.

  13. Multiresidue chromatographic method for the determination of macrolide residues in muscle by high-performance liquid chromatography with UV detection.

    PubMed

    Juhel-Gaugain, M; Anger, B; Laurentie, M

    1999-01-01

    A high-performance liquid chromatographic (HPLC) method for the simultaneous determination of tilmicosin, tylosin, spiramycin, and its major metabolite neospiramycin was developed that is suitable for porcine, bovine, and poultry muscles. Macrolide residues were extracted from muscle with acetonitrile, fat was removed by liquid-liquid extraction with isooctane, and the extract was then cleaned on Bond Elut C18 cartridges. The HPLC separation was performed on an Inertsil ODS3 C18 column (150 x 4 mm) with 0.05% trifluoroacetic acid-acetonitrile in a gradient mode. Two different chromatographic gradients were used for tilmicosin-tylosin and spiramycin-neospiramycin, and the detection wavelengths were 287 and 232 nm, respectively. The method was validated from 1/2 the maximum residue limit (MRL) to 4 times the MRL with pork muscle samples. Mean recoveries were 60, 63.5, 51, and 42% for tilmicosin, tylosin, spiramycin, and neospiramycin, respectively. The detection limits are 15 micrograms/kg for tilmicosin and tylosin, 30 micrograms/kg for spiramycin, and 25 micrograms/kg for neospiramycin. Linearity, precision, and accuracy of the method were also tested.

  14. Simple detection of residual enrofloxacin in meat products using microparticles and biochips.

    PubMed

    Ha, Mi-Sun; Chung, Myung-Sub; Bae, Dong-Ho

    2016-05-01

    A simple and sensitive method for detecting enrofloxacin, a major veterinary fluoroquinolone, was developed. Monoclonal antibody specific for enrofloxacin was immobilised on a chip and fluorescent dye-labelled microparticles were covalently bound to the enrofloxacin molecules. Enrofloxacin in solution competes with the microparticle-immobilised enrofloxacin (enroMPs) to bind to the antibody on the chip. The presence of enrofloxacin was verified by detecting the fluorescence of enrofloxacin-bound microparticles. Under optimum conditions, a high dynamic range was achieved at enrofloxacin concentrations ranging from 1 to 1000 μg kg(-1). The limits of detection and quantification for standard solutions were 5 and 20 μg kg(-1) respectively, which are markedly lower than the maximum residue limit. Using simple extraction methods, recoveries from fortified beef, pork and chicken samples were 43.4-62.3%. This novel method also enabled approximate quantification of enrofloxacin concentration: the enroMP signal intensity decreased with increasing enrofloxacin concentration. Because of its sensitivity, specificity, simplicity and rapidity, the method described herein will facilitate the detection and approximate quantification of enrofloxacin residues in foods in a high-throughput manner.

  15. Combination of QuEChERS and DLLME for GC-MS determination of pesticide residues in orange samples.

    PubMed

    Andraščíková, Mária; Hrouzková, Svetlana; Cunha, Sara C

    2013-01-01

    A new method combining QuEChERS (quick, easy, cheap, effective, rugged and safe) and DLLME (dispersive liquid-liquid microextraction) followed by gas chromatography-mass spectrometry with selected ion monitoring (SIM) was developed for the simultaneous determination of 19 pesticides from nine chemical groups exhibiting or suspected to exhibit endocrine-disrupting properties in orange samples. Acetonitrile extract obtained from QuEChERS extraction was used for DLLME as dispersive solvent and carbon tetrachloride as extractive solvent to increase the enrichment factor of the extraction procedure. The effect of several extraction parameters, such as volume extract achieved by the QuEChERS method and subsequently used for DLLME, selection of extractive solvent and its volume, was tested. Under optimum conditions, good linearity, satisfactory recoveries and repeatability were obtained. Limits of quantification (LOQs) achieved (ranging from 0.02 to 47 ng/g) were below the maximum residue limits established by the European Union. The proposed method was applied to the monitoring of pesticide residue levels in oranges commercialised in Portugal.

  16. Determination of 28 pesticides applied on two tomato cultivars with a different surface/weight ratio of the berries, using a multiresidue GC-MS/MS method.

    PubMed

    Dedola, Fabrizio; Cabizza, Maddalena; Satta, Maurizio

    2014-01-01

    The behavior of 28 pesticides on two tomato cultivars with a different surface/weight (S/W) ratio of the berries (S/W, Birikino vs. Tombola) was studied, in order to provide appropriate indications about their persistence on crops reaching the pre-harvest interval (PHI). Quantitative analysis was performed using a GC MS/MS method. Birikino cv. (BIR) was a "cherry type tomato" with a double S/W ratio compared with Tombola cv. (TOM). The results showed a different pesticide behavior. Azoxystrobin, Boscalid, Bupirimate, Difenoconazole, Etofenprox, Iprodione, Mepanipyrim, Myclobutanil, Tebuconazole, Zoxamide, Metalaxyl M, Pyrimethanil, Tetraconazole, Benalaxyl, Cyprodinil, Fenamidone, Famoxadone and Fludioxonil immediately after treatments showed residues on BIR higher than TOM, and this behavior is consistent with its greater exposed surface. BIR showed higher decay rates of these pesticides during the whole trial, nevertheless residue averages remained higher than TOM reaching the time of harvest. Residues at the PHI were all below their Maximum Residue Levels (MRLs), but data indicated that they could exceed their legal limits especially if the above-mentioned active ingredients were employed more than once per crop cycle on cherry type tomatoes. As regards to Chlorpyrifos, Chlorpyrifos methyl, Triadimenol, Pyridaben and Tebufenpyrad, no different residual behavior related to S/W ratio of the cultivars was observed. Even in this case, residues at the PHI were all below MRLs. As for Cyfluthrin, Deltamethrin, Lambda cyhalothrin, Etoxazole and Cyproconazole, residues were lower than the limit of quantitation (LOQ) of the analytical method just after the treatment, according to their low doses of employment.

  17. Ultrasonically Modified Amended-Cloud Point Extraction for Simultaneous Pre-Concentration of Neonicotinoid Insecticide Residues.

    PubMed

    Kachangoon, Rawikan; Vichapong, Jitlada; Burakham, Rodjana; Santaladchaiyakit, Yanawath; Srijaranai, Supalax

    2018-05-12

    An effective pre-concentration method, namely amended-cloud point extraction (CPE), has been developed for the extraction and pre-concentration of neonicotinoid insecticide residues. The studied analytes including clothianidin, imidacloprid, acetamiprid, thiamethoxam and thiacloprid were chosen as a model compound. The amended-CPE procedure included two cloud point processes. Triton™ X-114 was used to extract neonicotinoid residues into the surfactant-rich phase and then the analytes were transferred into an alkaline solution with the help of ultrasound energy. The extracts were then analyzed by high-performance liquid chromatography (HPLC) coupled with a monolithic column. Several factors influencing the extraction efficiency were studied such as kind and concentration of surfactant, type and content of salts, kind and concentration of back extraction agent, and incubation temperature and time. Enrichment factors (EFs) were found in the range of 20⁻333 folds. The limits of detection of the studied neonicotinoids were in the range of 0.0003⁻0.002 µg mL −1 which are below the maximum residue limits (MRLs) established by the European Union (EU). Good repeatability was obtained with relative standard deviations lower than 1.92% and 4.54% for retention time ( t R ) and peak area, respectively. The developed extraction method was successfully applied for the analysis of water samples. No detectable residues of neonicotinoids in the studied samples were found.

  18. Maximum residue level validation of triclabendazole marker residues in bovine liver, muscle and milk matrices by ultra high pressure liquid chromatography tandem mass spectrometry.

    PubMed

    Whelan, Michelle; O'Mahony, John; Moloney, Mary; Cooper, Kevin M; Furey, Ambrose; Kennedy, D Glenn; Danaher, Martin

    2013-02-01

    Triclabendazole is the only anthelmintic drug, which is active against immature, mature and adult stages of fluke. The objective of this work was to develop an analytical method to quantify and confirm the presence of triclabendazole residues around the MRL. In this work, a new analytical method was developed, which extended dynamic range to 1-100 and 5-1000 μg kg(-1) for milk and tissue, respectively. This was achieved using a mobile phase containing trifluoroacetic acid (pK(a) of 0.3), which resulted in the formation of the protonated pseudomolecular ions, [M+H](+), of triclabendazole metabolites. Insufficient ionisation of common mobile phase additives due to low pK(a) values (<2) was identified as the cause of poor linearity. The new mobile phase conditions allowed the analysis of triclabendazole residues in liver, muscle and milk encompassing their EU maximum residue levels (MRL) (250, 225 and 10 μg kg(-1) respectively). Triclabendazole residues were extracted using a modified QuEChERS method and analysed by positive electrospray ionisation mass spectrometry with all analytes eluted by 2.23 min. The method was validated at the MRL according to Commission Decision (CD) 2002/657/EC criteria. The decision limit (CCα) of the method was in the range of 250.8-287.2, 2554.9-290.8 and 10.9-12.1 μg kg(-1) for liver, muscle and milk, respectively. The performance of the method was successfully verified for triclabendazole in muscle by participating in a proficiency study, the method was also applied to incurred liver, muscle and milk samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. Dissipation pattern of flubendiamide residues on capsicum fruit (Capsicum annuum L.) under field and controlled environmental conditions.

    PubMed

    Buddidathi, Radhika; Mohapatra, Soudamini; Siddamallaiah, Lekha; Manikrao, Gourishankar; Hebbar, Shibara Shankara

    2016-01-01

    This investigation was undertaken to compare the dissipation pattern of flubendiamide in capsicum fruits under poly-house and open field after giving spray applications at the recommended and double doses of 48 g a.i. ha(-1) and 96 g a.i. ha(-1). Extraction and purification of capsicum fruit samples were carried out by the QuEChERS method. Residues of flubendiamide and its metabolite, des-iodo flubendiamide, were analyzed by high-performance liquid chromatography-photodiode array, and confirmed by liquid chromatography-mass spectrometry/mass spectrometry. Limit of quantification of the method was 0.05 mg kg(-1), and recovery of the insecticides was in the range of 89.6-104.3%, with relative standard deviation being 4.5-11.5%. The measurement uncertainty of the analytical method was in the range of 10.7-15.7%. Initial residue deposits of flubendiamide on capsicum fruits grown under poly-house conditions were (0.977 and 1.834 mg kg(-1)) higher than that grown in the field (0.665 and 1.545 mg kg(-1)). Flubendiamide residues persisted for 15 days in field-grown and for 25 days in poly-house-grown capsicum fruits. The residues were degraded with the half-lives of 4.3-4.7 and 5.6-6.6 days in field and poly-house respectively. Des-iodo flubendiamide was not detected in capsicum fruits or soil. The residues of flubendiamide degraded to below the maximum residue limit notified by Codex Alimentarius Commission (FAO/WHO) after 1 and 6 days in open field, and 3 and 10 days in poly-house. The results of the study indicated that flubendiamide applied to capsicum under controlled environmental conditions required longer pre-harvest interval to allow its residues to dissipate to the safe level.

  20. Residue decline and risk assessment of fluopyram + tebuconazole (400SC) in/on onion (Allium cepa).

    PubMed

    Patel, Badal V; Chawla, Suchi; Gor, Hetal; Upadhyay, Payal; Parmar, Kaushik D; Patel, Anil R; Shah, Paresh G

    2016-10-01

    A method was validated for estimating fluopyram and tebuconazole in onion on LC-MS/MS using dispersive QuEChERS. Three sprays of a combination fungicide fluopyram + tebuconazole (Luna experience, 400 SC) were applied @ 75 + 75 and 150 + 150 g a.i. ha -1 at an interval of 10 days on onion using Knapsack sprayer. First spray was made at bulb setting stage. Spring onion samples were drawn at 0 (1 h), 1, 3, 5, 7, 10, 15, and 20 days and matured onion bulb at harvest (52 days) after the last spray. Soil samples were also drawn at harvest. Foliar application of the combination product resulted in 1.14 and 2.86 mg kg -1 fluopyram residues on spring onion at standard and double dose, respectively, one hour after the last application. The levels of fluopyram residues gradually declined and recorded 0.25 and 0.58 mg kg -1 on 20th day of application with half-lives of 8.8 and 9.1 days at standard and double dose, respectively. For tebuconazole, the corresponding residues observed after 1 h (0 day) of application were 0.92 and 2.29 mg kg -1 . The levels declined gradually to 0.12 and 0.33 mg kg -1 on 20th days with half-life of 6.7 to 7.7 days at standard and double dose, respectively. Here, we are proposing a pre-harvest interval of 7 day for fluopyram and tebuconazole in spring onion when applied at 75 + 75 g a.i. ha -1 (400 SC). Risk assessment was done by calculating hazard quotient and by comparing theoretical maximum residue intake (TMRI) with maximum permissible intake (MPI). In all the cases, results of the study showed that HQ (Hazard Quotient) ≤1 and TMDI < MPI. Hence, the use of this combination product can be recommended with pre harvest interval of 7 days. The data can be used in establishing MRLs (maximum residue limits) for spring onion after considering multilocation trials.

  1. Numerical Study of Mechanical Response of Pure Titanium during Shot Peening

    NASA Astrophysics Data System (ADS)

    Wang, Y. M.; Cheng, J. P.; Yang, H. P.; Zhang, C. H.

    2018-05-01

    Mechanical response of pure titanium impacted by a steel ball was simulated using finite element method to investigate stress and strain evolution during shot peening. It is indicated that biaxial residual stress was obtained in the surface layer while in the interior triaxial residual stress existed because the S33 was comparable to S11 and S22. With decreasing the depth from the top surface, the stress was higher during impacting, but the stress relief extent became more significant when the ball rebounded. Therefore the maximum residual stress was formed in the subsurface layer with depth of 130 μm. As for the residual strain, it is shown that the maximum residual strain LE33 was obtained at the depth of 60 μm corresponding to the maximum shear stress during impacting.

  2. Monitoring of Pesticide Residues in Commonly Used Fruits and Vegetables in Kuwait.

    PubMed

    Jallow, Mustapha F A; Awadh, Dawood G; Albaho, Mohammed S; Devi, Vimala Y; Ahmad, Nisar

    2017-07-25

    The presence of pesticide residues in primary and derived agricultural products raises serious health concerns for consumers. The aim of this study was to assess the level of pesticide residues in commonly consumed fruits and vegetables in Kuwait. A total of 150 samples of different fresh vegetables and fruits were analyzed for the presence of 34 pesticides using the quick easy cheap effective rugged and safe (QuEChERS) multi-residue extraction, followed by gas chromatography-mass spectrometry (GC-MS) or liquid chromatography-tandem mass spectrometry (LC - MS / MS). Pesticide residues above the maximum residue limits (MRL) were detected in 21% of the samples and 79% of the samples had no residues of the pesticides surveyed or contained residues below the MRL. Multiple residues were present in 40% of the samples with two to four pesticides, and four samples were contaminated with more than four pesticide residues. Of the pesticides investigated, 16 were detected, of which imidacloprid, deltamethrin, cypermethrin, malathion, acetamiprid, monocrotophos, chlorpyrifos-methyl, and diazinon exceeded their MRLs. Aldrin, an organochlorine pesticide, was detected in one apple sample, with residues below the MRL. The results indicate the occurrence of pesticide residues in commonly consumed fruits and vegetables in Kuwait, and pointed to an urgent need to develop comprehensive intervention measures to reduce the potential health risk to consumers. The need for the regular monitoring of pesticide residues and the sensitization of farmers to better pesticide safety practices, especially the need to adhere to recommended pre-harvest intervals is recommended.

  3. Levels of organophosphorus pesticides in medicinal plants commonly consumed in Iran

    PubMed Central

    2012-01-01

    The frequent occurrence of pesticide residues in herbal materials was indicated by previous studies. In this study, the concentration of some of the organophosphorus pesticides including parathion, malathion, diazinon and pirimiphos methyl in different kinds of medicinal plants were determined. The samples were collected randomly from ten local markets of different areas of Iran. At the detection limit of 0.5 ng g-1, parathion and pirimiphos methyl were not detected in any of the samples. Some amounts of malathion and diazinon were found in Zataria, Matricaria chamomile, Spearmint and Cumin Seed samples while, the concentrations of target organophosphorus pesticides in Borage samples were below the detection limits of the methods which could be a result of intensive transformation of organophosphorus pesticides by Borage. In addition the organophosphorus pesticides were detected in all of the samples below the maximum residue levels (MRLs) proposed by the international organizations. PMID:23351610

  4. Pesticides residues and metals in plant products from agricultural area of Belgrade, Serbia.

    PubMed

    Ethorđević, Tijana; Ethurović, Rada

    2012-03-01

    The objective of study was to assess the levels of selected metals and pesticides in plant products from agricultural area of Belgrade, Serbia in order to indicate their possible sources and risks of contamination and to evaluate their sanitary probity and safety. The concentrations of cadmium, copper, iron, manganese, nickel, lead and zinc were below limits established by national and international regulations (maximum found concentrations were 0.028, 1.91, 11.16, 1.77, 0.605, 0.073 and 1.76 mg kg(-1) respectively). Only residue of one of examined pesticides was found in amount below MRL (bifenthrin 2.46 μg kg(-1)) in only one of analysed samples, while others were below detection limits. Obtained results indicate that crops from examined agricultural areas are unpolluted by contaminants used for plant protection and nutrition, indicating good agricultural practice regarding pesticides and fertilizer usage as well as moderate industrial production within examined areas.

  5. Consumer exposure to pesticide residues in apples from the region of south-eastern Poland.

    PubMed

    Szpyrka, Ewa; Kurdziel, Anna; Słowik-Borowiec, Magdalena; Grzegorzak, Magdalena; Matyaszek, Aneta

    2013-11-01

    The production of apples in Poland is the largest among the countries of the European Union, and therefore, the consumption of these fruits is high in our country. The aim of this study was to determine the presence of pesticide residues in Polish apples and to assess if these residues pose a risk to the health of the consumer. Furthermore, compliance with legal regulations concerning the use of plant protection products in crop cultivation was ascertained. Pesticide residues were found in 192 samples (61.5% of tested samples). In six samples (1.9%), residues exceeded maximum residue limits. Violations concerned the insecticides: indoxacarb, diazinon and fenitrothion. The highest long-term consumer exposure was found in the case of consumption of apples with diazinon residue for both groups, adults and toddlers [4% acceptable daily intake (ADI), adults; 21% ADI, toddlers]. The highest values of short-term exposure were obtained in the case of consumption of apples with indoxacarb [5% acute reference dose (ARfD), adults; 27% ARfD, toddlers] and fenitrothion (4% ARfD, adults; 23% ARfD, toddlers). Although fungicides are the pesticides found most often in apples, the consumption of apples with insecticide residues constitutes the greatest hazard to human health.

  6. 40 CFR 180.545 - Prallethrin (RS)-2-methyl-4-oxo-3-(2-propynyl)cyclopent-2-enyl (1RS)-cis, trans-chrysanthemate...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... shall be limited to a maximum of 2.0% active ingredient. Contamination of food or food contact surfaces... EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Specific Tolerances § 180.545 Prallethrin (RS)-2-methyl-4...-methyl-4-oxo-3-(2-propynyl)cyclopent-2-enyl (1RS)-cis, trans-chrysanthemate as follows: (2) In or on food...

  7. A Survey of Naturally-Occurring Steroid Hormones in Raw Milk and the Associated Health Risks in Tangshan City, Hebei Province, China

    PubMed Central

    Qu, Xueyin; Su, Chuanyou; Zheng, Nan; Li, Songli; Meng, Lu; Wang, Jiaqi

    2017-01-01

    In recent years, high levels of hormone residue in food, capable of damaging the health of consumers, have been recorded frequently. In this study, 195 raw milk samples were obtained from Tangshan City, China, and the concentrations of 22 steroid hormones were measured by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Cortisol was detected in 12.5% of raw milk samples (mean 0.61 µg/kg; range:

  8. Survey of pesticide residues in maize, cowpea and millet from northern Cameroon: part I.

    PubMed

    Sonchieu, Jean; Benoit Ngassoum, Martin; Bosco Tchatchueng, Jean; Srivastava, Ashutosh Kumar; Srivastava, Laxman Prasad

    2010-01-01

    In northern Cameroon, the misuse of pesticides for pest control is common among small-scale farmers. Therefore, monitoring of pesticide residues was carried out on stored maize, cowpea and millet from eight localities. The determination of residues of organochlorines (lindane, α-endosulfan and β-endosulfan), organophosphorus compounds (malathion and pirimiphos-methyl), synthetic pyrethroids (permethrin) and carbamates (carbufuran) was performed using GC-ECD/NPD and GC-MS for confirmation. Organochlorine pesticides were detected more frequently and in higher concentrations, ranging from 0.02 ± 0.01 mg kg(-1) for β-endosulfan in millet to 9.53 ± 4.00 mg kg(-1) lindane in maize, than organophosphorus compounds, with concentrations varying from 0.04 ± 0.03 mg kg(-1) for pirimiphos methyl to 0.23 ± 0.38 mg kg(-1) for malathion in maize. Permethrin was found only in maize at 0.39 ± 0.23 mg kg(-1). No carbofuran was found. More than 75% of samples contained pesticide residues above the maximum residue limit (MRL); showing a potential human dietary risk related to consumption of these grains.

  9. Effectiveness of stress release geometries on reducing residual stress in electroforming metal microstructure

    NASA Astrophysics Data System (ADS)

    Song, Chang; Du, Liqun; Zhao, Wenjun; Zhu, Heqing; Zhao, Wen; Wang, Weitai

    2018-04-01

    Micro electroforming, as a mature micromachining technology, is widely used to fabricate metal microdevices in micro electro mechanical systems (MEMS). However, large residual stress in the local positions of the micro electroforming layer often leads to non-uniform residual stress distributions, dimension accuracy defects and reliability issues during fabrication of the metal microdevice. To solve this problem, a novel design method of presetting stress release geometries in the topological structure of the metal microstructure is proposed in this paper. First, the effect of stress release geometries (circular shape, annular groove shape and rivet shape) on the residual stress in the metal microstructure was investigated by finite element modeling (FEM) analysis. Two evaluation parameters, stress concentration factor K T and stress non-uniformity factor δ were calculated. The simulation results show that presetting stress release geometries can effectively reduce and homogenize the residual stress in the metal microstructures were measured metal microstructure. By combined use with stress release geometries of annular groove shape and rivet shape, the stress concentration factor K T and the stress non-uniformity factor δ both decreased at a maximum of 49% and 53%, respectively. Meanwhile, the average residual stress σ avg decreased at a maximum of 20% from  -292.4 MPa to  -232.6 MPa. Then, micro electroforming experiments were carried out corresponding to the simulation models. The residual stresses in the metal microstructures were measured by micro Raman spectroscopy (MRS) method. The results of the experiment proved that the stress non-uniformity factor δ and the average residual stress σ avg also decreased at a maximum with the combination use of annular groove shape and rivet shape stress release geometries, which is in agreement with the results of FEM analysis. The stress non-uniformity factor δ has a maximum decrease of 49% and the average residual stress σ avg has a maximum decrease of 37% from  -257.0 MPa to  -162.0 MPa.

  10. Tissue residue depletion of moxidectin in lambs (Ovis aries) following subcutaneous administration.

    PubMed

    Cruz, Michelle Del Bianchi A; Fernandes, Maria Ângela M; Monteiro, Alda Lúcia G; Teles, Juliana A; Anadón, Arturo; Reyes, Felix G R

    2018-06-07

    To date, a tissue depletion study of moxidectin (MOX) in lambs is not available. Thus, considering that lamb meat is of great commercial interest in the world, the aim of the present study was to determine the residue levels of MOX in lamb target-tissues (muscle, liver, kidney and fat) and subsequently calculate the MOX withdrawal period. For this purpose, the target-tissues were analysed by ultra-high-performance liquid chromatography-tandem mass spectrometry. Method validation was performed based on Commission Decision 2002/657/EC and VICH GL49. To quantify the analyte, matrix-matched analytical curves were constructed with spiked blank tissues. The limits of detection and quantitation were 1.5 and 5 ng g -1 , respectively, for all matrices. The linearity, decision limit, detection capability accuracy and inter- and intra-day precision of the method are reported. The lambs were treated with a single subcutaneous dose of 0.2 mg MOX kg -1 body weight and were slaughtered in accordance with accepted animal care protocols. Samples of target-tissues were collected on 2, 4, 7, 14, 28 and 42 days after MOX administration. During the whole study, the highest drug residue level occurred in the fat. For the other target-tissues (muscle, liver and kidney), MOX concentrations were below the maximum residue limit (MRL). Considering the MRL value of 500 µg kg -1 for MOX residues in sheep fat, our results in lambs allowed the estimation of a MOX withdrawal period of 31 days. This indicates that the withdrawal period established for MOX in adult sheep (28 days) does not apply for lambs.

  11. Persistence of α-cypermethrin residues in milk of lactating donkeys (Equus asinus) using UHPLC-MS/MS.

    PubMed

    Chirollo, Claudia; Radovnikovic, Anita; Veneziano, Vincenzo; Marrone, Raffaele; Pepe, Tiziana; Danaher, Martin; Anastasio, Aniello

    2014-01-01

    The aim of this study was to measure the persistence of residues of the pyrethroid insecticide α-cypermethrin (ACYP) in the milk of lactating donkeys following pour-on treatment. Milk was collected from animals (n = 7) before the treatment and at 12, 24, 36, 48, 60, 72 and 84 h post-treatment. The last sampling was taken 7 days post-treatment (168 h). Milk samples were analysed by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). The analytical method was validated following requirements of Commission Decision 2002/657/EC. All samples showed levels of ACYP below the maximum residue limit (MRL) of 20 μg kg(-1) established for bovine milk (Commission Regulation (EU) No. 37/2010). The results demonstrate that there is minimal partitioning of ACYP into milk in lactating donkeys from pour-on treatment.

  12. Determination of pesticides in coconut (Cocos nucifera Linn.) water and pulp using modified QuEChERS and LC-MS/MS.

    PubMed

    Ferreira, Jordana Alves; Ferreira, Joana Maria Santos; Talamini, Viviane; Facco, Janice de Fátima; Rizzetti, Tiele Medianeira; Prestes, Osmar Damian; Adaime, Martha Bohrer; Zanella, Renato; Bottoli, Carla Beatriz Grespan

    2016-12-15

    The use of pesticides is directly linked to improvements in productivity and to the preservation of coconut palms. However pesticide analysis is necessary to determine whether pesticide residues in the food products containing coconut are within the maximum residue limits (MRLs), ensuring the quality of these products. This work aimed to develop a method for multiresidue determination of ten pesticides in coconut water and pulp using QuEChERS and LC-MS/MS. The method was effective in terms of selectivity, linearity, matrix effect, accuracy and precision, providing LOD of 3μgkg(-1), LOQ of 10μgkg(-1) and recoveries between 70 and 120% with RSD lower than 20%. The developed method was applied to 36 samples in which residues of carbendazim, carbofuran, cyproconazole and thiabendazole were found below the LOQ in coconut water and pulp. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Acetylcholinesterase Immobilized on Magnetic Beads for Pesticides Detection: Application to Olive Oil Analysis

    PubMed Central

    Ben Oujji, Najwa; Bakas, Idriss; Istamboulié, Georges; Ait-Ichou, Ihya; Ait-Addi, Elhabib; Rouillon, Régis; Noguer, Thierry

    2012-01-01

    This work presents the development of bioassays and biosensors for the detection of insecticides widely used in the treatment of olive trees. The systems are based on the covalent immobilisation of acetylcholinesterase on magnetic microbeads using either colorimetry or amperometry as detection technique. The magnetic beads were immobilised on screen-printed electrodes or microtitration plates and tested using standard solutions and real samples. The developed devices showed good analytical performances with limits of detection much lower than the maximum residue limit tolerated by international regulations, as well as a good reproducibility and stability. PMID:22969377

  14. Determination of organophosphorus pesticide residues in vegetables by an enzyme inhibition method using α-naphthyl acetate esterase extracted from wheat flour*

    PubMed Central

    Wang, Jun-liang; Xia, Qing; Zhang, An-ping; Hu, Xiao-yan; Lin, Chun-mian

    2012-01-01

    The widespread use of organophosphorus pesticides (OPs) poses a great threat to human health and has made the detection of OP residues in food an important task, especially in view of the fact that easy and rapid detection methods are needed. Because OPs have inhibitory effects on the activity of α-naphthyl acetate esterase (ANAE) in plants, in this work we evaluated the possibility of detecting OPs in vegetables with ANAE extracted from commercial flour. The limits of detection (LODs) obtained for methamidophos, dichlorvos, phoxim, dimethoate, and malathion in lettuce samples with crude ANAE were 0.17, 0.11, 0.11, 0.96, and 1.70 mg/kg, respectively. Based on the maximum residue limits (MRLs) for OPs in food stipulated by Chinese laws which are 0.05, 0.20, 0.05, 1.00, and 8.00 mg/kg for methamidophos, dichlorvos, phoxim, dimethoate, and malathion, respectively, the esterase inhibition method with crude ANAE had sufficient sensitivity to detect the residues of dichlorvos, dimethoate, and malathion in lettuce, but it could not be used to guarantee the safety of the same samples if methamidophos or phoxim residue was present. The sensitivity of the method was improved by the use of esterase purified by ammonium sulfate salting-out. The LODs obtained for methamidophos and phoxim with purified esterase were lower than the MRLs for these OPs in food. This is a very promising method for the detection of OP residues in vegetables using crude or purified esterase because of its cheapness, sensitivity, and convenience. PMID:22467368

  15. Residue level and dissipation pattern of lepimectin in shallots using high-performance liquid chromatography coupled with photodiode array detection.

    PubMed

    Kim, Sung-Woo; Rahman, Md Musfiqur; Abd El-Aty, A M; Truong, Lieu T B; Choi, Jeong-Heui; Park, Joon-Seong; Kim, Mi-Ra; Shin, Ho-Chul; Shim, Jae-Han

    2016-11-01

    Lepimectin, as an emulsifiable concentrate, was sprayed on shallots at the recommended dose rate (10 mL/20 L) to determine its residue levels, dissipation pattern, pre-harvest residue limits (PHRLs), and health risk. Samples were randomly collected over 10 days, extracted with acetonitrile, purified using an amino solid-phase extraction (NH 2 -SPE) cartridge and analyzed using a high-performance liquid chromatography-photodiode array detection method. Field-incurred samples were confirmed using ultra-performance liquid chromatography-tandem mass spectrometry. The linearity was excellent, with a determination coefficient (R 2 ) of ≥0.9991. The recoveries at two spiking levels (0.2 and 1.0 mg/kg) ranged from 84.49 to 87.64% with relative standard deviations of ≤7.04%. The developed method was applied to field samples grown in separate greenhouses, one located in Naju and one in Muan, in the Republic of Korea. The dissipation pattern was described by first-order kinetics with half-lives of 1.9 (Naju) and 1.7 days (Muan). The PHRL curves indicated that, if the lepimectin residues are <0.18 (Naju) and <0.13 mg/kg (Muan) 5 days before harvest, the residue levels will be lower than the maximum residue limit (0.05 mg/kg) upon harvesting. The risk assessment data indicated that lepimectin is safe for use in the cultivation of shallots, with no risk of detrimental effects to the consumer. Copyright © 2016 John Wiley & Sons, Ltd.

  16. Residue level and dissipation of carbendazim in/on pomegranate fruits and soil.

    PubMed

    Mohapatra, Soudamini; S, Lekha

    2016-07-01

    Carbendazim is widely used on pomegranate for control of a large number of fungal diseases. Its residue levels in/on pomegranate fruits and soil were evaluated under field conditions. The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method in conjunction with liquid-chromatography mass spectrometry was used for analysis of carbendazim. Recovery of carbendazim was within 78.92-96.28 % and relative standard deviation within 3.8-10.9 % (n = 6). Carbendazim residues on pomegranate fruits dissipated at the half lives of 17.3 and 22.8 days from treatments at 500 and 1000 g active ingredient (a.i.) ha(-1), respectively. Its residues in pomegranate aril were highest on the tenth day and reduced thereafter. The residue level of carbendazim on pomegranate whole fruits from standard dose treatment was less than the EU maximum residue limit (MRL) of 0.1 mg kg(-1) at harvest. The carbendazim residues were

  17. Pesticide residues in Portuguese strawberries grown in 2009-2010 using integrated pest management and organic farming.

    PubMed

    Fernandes, Virgínia C; Domingues, Valentina F; Mateus, Nuno; Delerue-Matos, Cristina

    2012-11-01

    Pesticides are among the most widely used chemicals in the world. Because of the widespread use of agricultural chemicals in food production, people are exposed to low levels of pesticide residues through their diets. Scientists do not yet have a total understanding of the health effects of these pesticide residues. This work aims to determine differences in terms of pesticide residue content in Portuguese strawberries grown using different agriculture practices. The Quick, Easy, Cheap, Effective, Rugged, and Safe sample preparation method was conducted and shown to have good performance for multiclass pesticides extraction in strawberries. The screening of 25 pesticides residue was performed by gas chromatography-tandem mass spectrometry. In quantitative validation, acceptable performances were achieved with recoveries of 70-120 and <12 % residual standard deviation for 25 pesticides. Good linearity was obtained for all the target compounds, with highly satisfactory repeatability. The limits of detection were in the range of 0.1-28 μg/kg. The method was applied to analyze strawberry samples from organic and integrated pest management (IPM) practices harvested in 2009-2010. The results showed the presence of fludioxonil, bifenthrin, mepanipyrim, tolylfluanid, cyprodinil, tetraconazole, and malathion when using IPM below the maximum residue levels.

  18. Effect of processing on the disappearance of pesticide residues in fresh-cut lettuce: Bioavailability and dietary risk.

    PubMed

    Camara, Miguel A; Barba, Alberto; Cermeño, Sandra; Martinez, Gracia; Oliva, Jose

    2017-12-02

    The aim of this research is to establish the processing factors of six pesticides durong the preparation of fresh-cut lettuce and to assess the risk of ingestion of pesticide residues associated with the consumption of the same. A field study was carried out on the dissipation of three insecticides (imidacloprid, tebufenozide, cypermethrin) and three fungicides (metalaxyl, tebuconazole, azoxystrobin) during treatment conditions simulating those used for commercial fresh-cut lettuce. A simultaneous residue analysis method is validated using QuEChERS extraction with acetonitrile and CG-MS and LC-MS/MS analysis. The residues detected after field application never exceed the established Maximum Residue Limits. The processing factors were generally less than 1 (between 0.34 for tebufenozide and 0.53 for imidacloprid), indicating that the process, as a whole, considerably reduces residue levels in processed lettuce compared to fresh lettuce. It is confirmed that cutting, followed by washing and drying, considerably reduces the residues. A matrix effect in the dialyzation of the pesticides is observed and the in vitro study of bioavailability establishes a low percentage of stomach absorption capacity (<15%). The EDI/ADI ratios found in all cases were well below their ADI values, and the dietary exposure assessed (EDI) in fresh-cut lettuce showed no concerns for consumer health.

  19. Residues of aflatoxin B1 in broiler meat: effect of age and dietary aflatoxin B1 levels.

    PubMed

    Hussain, Zahid; Khan, Muhammad Zargham; Khan, Ahrar; Javed, Ijaz; Saleemi, Muhammad Kashif; Mahmood, Sultan; Asi, Muhammad Rafique

    2010-12-01

    This study describes the effect of dietary levels of aflatoxin B1 (AFB1) and age of the birds upon the residue level in liver and muscles of broiler chicks. In three different experiments broiler chicks of 7, 14 and 28 days of age were kept for 7 days on contaminated rations having 1600, 3200 and 6400 μg/kg AFB1. AFB1 residues were detected earlier in younger birds and those fed high AFB1 dietary levels. The highest residue levels in liver and muscles of young chicks fed 6400 μg/kg AFB1 was 6.97±0.08 and 3.27±0.05 ng/g, respectively. Maximum residue concentration was high in birds of young age and those kept on high AFB1 ration. After withdrawal of AF contaminated rations, residues clearance was slow and AFB1 was detectable in liver and muscles of birds for longer duration in younger birds and those fed high AFB1 dietary levels. AFB1 residues in poultry tissues may buildup to high levels in areas with no regulatory limits on AFB1 levels of poultry feed and may pose a risk to consumers health. Copyright © 2010 Elsevier Ltd. All rights reserved.

  20. Simultaneous analysis of coccidiostats and sulfonamides in non-target feed by HPLC-MS/MS and validation following the Commission Decision 2002/657/EC.

    PubMed

    Gavilán, Rosa Elvira; Nebot, Carolina; Patyra, Ewelina; Miranda, Jose Manuel; Franco, Carlos Manuel; Cepeda, Alberto

    2018-05-02

    Taking into consideration the maximum level for coccidiostats included in the European Regulation 574/2011 and the fact that the presence of residues of sulfonamides in non-target feed is forbidden, the aim of this article is to present an analytical method based on HPLC-MS/MS for the identification and quantification of sulfonamides and coccidiostats in non-target feeds. The method was validated following Decision 2002/657/EC and recovery, repeatability, and reproducibility were within the limits stablished in the Decision. For coccidiostats, the decision limit and detection capability were calculated for the different species taking into account the maximum level allowed in Regulation 574/2011. The applicability of the method was investigated in 50 feed samples collected from dairy farms, 50 obtained from feed mills, and 10 interlaboratory feed samples.

  1. A fundamental reconsideration of the CRASH3 damage analysis algorithm: the case against uniform ubiquitous linearity between BEV, peak collision force magnitude, and residual damage depth.

    PubMed

    Singh, Jai

    2013-01-01

    The objective of this study was a thorough reconsideration, within the framework of Newtonian mechanics and work-energy relationships, of the empirically interpreted relationships employed within the CRASH3 damage analysis algorithm in regards to linearity between barrier equivalent velocity (BEV) or peak collision force magnitude and residual damage depth. The CRASH3 damage analysis algorithm was considered, first in terms of the cases of collisions that produced no residual damage, in order to properly explain the damage onset speed and crush resistance terms. Under the modeling constraints of the collision partners representing a closed system and the a priori assumption of linearity between BEV or peak collision force magnitude and residual damage depth, the equations for the sole realistic model were derived. Evaluation of the work-energy relationships for collisions at or below the elastic limit revealed that the BEV or peak collision force magnitude relationships are bifurcated based upon the residual damage depth. Rather than being additive terms from the linear curve fits employed in the CRASH3 damage analysis algorithm, the Campbell b 0 and CRASH3 AL terms represent the maximum values that can be ascribed to the BEV or peak collision force magnitude, respectively, for collisions that produce zero residual damage. Collisions resulting in the production of non-zero residual damage depth already account for the surpassing of the elastic limit during closure and therefore the secondary addition of the elastic limit terms represents a double accounting of the same. This evaluation shows that the current energy absorbed formulation utilized in the CRASH3 damage analysis algorithm extraneously includes terms associated with the A and G stiffness coefficients. This sole realistic model, however, is limited, secondary to reducing the coefficient of restitution to a constant value for all cases in which the residual damage depth is nonzero. Linearity between BEV or peak collision force magnitude and residual damage depth may be applicable for particular ranges of residual damage depth for any given region of any given vehicle. Within the modeling construct employed by the CRASH3 damage algorithm, the case of uniform and ubiquitous linearity cannot be supported. Considerations regarding the inclusion of internal work recovered and restitution for modeling the separation phase change in velocity magnitude should account for not only the effects present during the evaluation of a vehicle-to-vehicle collision of interest but also to the approach taken for modeling the force-deflection response for each collision partner.

  2. Parametric study on single shot peening by dimensional analysis method incorporated with finite element method

    NASA Astrophysics Data System (ADS)

    Wu, Xian-Qian; Wang, Xi; Wei, Yan-Peng; Song, Hong-Wei; Huang, Chen-Guang

    2012-06-01

    Shot peening is a widely used surface treatment method by generating compressive residual stress near the surface of metallic materials to increase fatigue life and resistance to corrosion fatigue, cracking, etc. Compressive residual stress and dent profile are important factors to evaluate the effectiveness of shot peening process. In this paper, the influence of dimensionless parameters on maximum compressive residual stress and maximum depth of the dent were investigated. Firstly, dimensionless relations of processing parameters that affect the maximum compressive residual stress and the maximum depth of the dent were deduced by dimensional analysis method. Secondly, the influence of each dimensionless parameter on dimensionless variables was investigated by the finite element method. Furthermore, related empirical formulas were given for each dimensionless parameter based on the simulation results. Finally, comparison was made and good agreement was found between the simulation results and the empirical formula, which shows that a useful approach is provided in this paper for analyzing the influence of each individual parameter.

  3. Multiresidue determination of fluoroquinolone, sulfonamide, trimethoprim, and chloramphenicol antibiotics in urban waters in China.

    PubMed

    Peng, Xianzhi; Tan, Jianhua; Tang, Caiming; Yu, Yiyi; Wang, Zhendi

    2008-01-01

    A feasible method has been optimized to simultaneously determine multiclass antibiotic residues, including sulfonamides, fluoroquinolones, trimethoprim, and chloramphenicol in urban riverine water and wastewater by off-line solid phase extraction and high-performance liquid chromatography coupled with a diode-array ultraviolet detector and a fluorescence detector. Internal standard and standard addition methods were used in combination to identify and quantify these antibiotics to compensate for the matrix interference. The method quantification limits (MQLs) were determined to be 0.035 to 0.100 microg/L and 0.100 to 0.300 microg/L for the riverine water and wastewater, respectively. Recoveries of the investigated antibiotics ranged from 63 to 126%. Sulfamethoxazole was the most frequently detected antibiotic residue in Guangzhou section of the Major Pearl River, South China, with a maximum level of 0.510 microg/L. Fluoroquinolone antibiotics were relatively less detected with a maximum level of 0.459 microg/L. The maximum concentration of sulfamethoxazole reached 5.597 microg/L in the raw wastewater from a large-scale sewage treatment plant in Guangzhou city. Around 30% of sulfamethoxazole might survive the primary clarification and biotreatment processes in the sewage treatment plant. None of the investigated antibiotics have been found above MQLs in the final effluent after chlorine disinfection.

  4. Laser quench hardening of steel: Effects of superimposed elastic pre-stress on the hardness and residual stress distribution

    NASA Astrophysics Data System (ADS)

    Meserve, Justin

    Cold drawn AISI 4140 beams were LASER surface hardened with a 2 kW CO2 LASER. Specimens were treated in the free state and while restrained in a bending fixture inducing surface tensile stresses of 94 and 230 MPa. Knoop hardness indentation was used to evaluate the through thickness hardness distribution, and a layer removal methodology was used to evaluate the residual stress distribution. Results showed the maximum surface hardness attained was not affected by pre-stress during hardening, and ranged from 513 to 676 kg/mm2. The depth of effective hardening varied at different magnitudes of pre-stress, but did not vary proportionately to the pre-stress. The surface residual stress, coinciding with the maximum compressive residual stress, increased as pre-stress was increased, from 1040 MPa for the nominally treated specimens to 1270 MPa for specimens pre-stressed to 230 MPa. The maximum tensile residual stress observed in the specimens decreased from 1060 MPa in the nominally treated specimens to 760 MPa for specimens pre-stressed to 230 MPa. Similarly, thickness of the compressive residual stress region increased and the depth at which maximum tensile residual stress occurred increased as the pre-stress during treatment was increased Overall, application of tensile elastic pre-stress during LASER hardening is beneficial to the development of compressive residual stress in AISI 4140, with minimal impact to the hardness attained from the treatment. The newly developed approach for LASER hardening may support efforts to increase both the wear and fatigue resistance of parts made from hardenable steels.

  5. Organochlorine pesticide residues in strawberries from integrated pest management and organic farming.

    PubMed

    Fernandes, Virginia C; Domingues, Valentina F; Mateus, Nuno; Delerue-Matos, Cristina

    2011-07-27

    A rapid, specific, and sensitive method based on the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method and a cleanup using dispersive solid-phase extraction with MgSO(4), PSA, and C18 sorbents has been developed for the routine analysis of 14 pesticides in strawberries. The analyses were performed by three different analytical methodologies: gas chromatography (GC) with electron capture detection (ECD), mass spectrometry (MS), and tandem mass spectrometry (MS/MS). The recoveries for all the pesticides studied were from 46 to 128%, with relative standard deviation of <15% in the concentration range of 0.005-0.250 mg/kg. The limit of detection (LOD) for all compounds met maximum residue limits (MRL) accepted in Portugal for organochlorine pesticides (OCP). A survey study of strawberries produced in Portugal in the years 2009-2010 obtained from organic farming (OF) and integrated pest management (IPM) was developed. Lindane and β-endosulfan were detected above the MRL in OF and IPM. Other OCP (aldrin, o,p'-DDT and their metabolites, and methoxychlor) were found below the MRL. The OCP residues detected decreased from 2009 to 2010. The QuEChERS method was successfully applied to the analysis of strawberry samples.

  6. Qualitative and Quantitative Drug residue analyses: Florfenicol in white-tailed deer (Odocoileus virginianus) and supermarket meat by liquid chromatography tandem-mass spectrometry.

    PubMed

    Anderson, Shanoy C; Subbiah, Seenivasan; Gentles, Angella; Austin, Galen; Stonum, Paul; Brooks, Tiffanie A; Brooks, Chance; Smith, Ernest E

    2016-10-15

    A method for confirmation and detection of Florfenicol amine residues in white-tailed deer tissues was developed and validated in our laboratory. Tissue samples were extracted with ethyl acetate and cleaned up on sorbent (Chem-elut) cartridges. Liguid chromatography (LC) separation was achieved on a Zorbax Eclipse plus C18 column with gradient elution using a mobile phase composed of ammonium acetate in water and methanol at a flow rate of 300μL/min. Qualitative and quantitative analyses were carried out using liquid chromatography - heated electrospray ionization(HESI) and atmospheric pressure chemical ionization (APCI)-tandem mass spectrometry in the multiple reaction monitoring (MRM) interface. The limits of detection (LODs) for HESI and APCI probe were 1.8ng/g and 1.4ng/g respectively. Limits of quantitation (LOQs) for HESI and APCI probe were 5.8ng/g and 3.4ng/g respectively. Mean recovery values ranged from 79% to 111% for APCI and 30% to 60% for HESI. The validated method was used to determine white-tailed deer florfenicol tissue residue concentration 10-days after exposure. Florfenicol tissue residues concentration ranged from 0.4 to 0.6μg/g for liver and 0.02-0.05μg/g for muscle and a trace in blood samples. The concentration found in the tested edible tissues were lower than the maximum residual limit (MRL) values established by the federal drug administration (FDA) for bovine tissues. In summary, the resulting optimization procedures using the sensitivity of HESI and APCI probes in the determination of florfenicol in white-tailed deer tissue are the most compelling conclusions in this study, to the extent that we have applied this method in the evaluation of supermarket samples drug residue levels as a proof of principle. Copyright © 2016. Published by Elsevier B.V.

  7. Removal of fluoride, arsenic and coliform bacteria by modified homemade filter media from drinking water.

    PubMed

    Devi, Rani; Alemayehu, Esayas; Singh, Vijender; Kumar, Ashok; Mengistie, Embialle

    2008-05-01

    An attempt was made to investigate the removal of fluoride, arsenic and coliform bacteria from drinking water using modified homemade filter media. Batch mode experimental study was conducted to test the efficiency of modified homemade filter for reduction of impurities under the operating condition of treatment time. The physico-chemical and biological analysis of water samples had been done before and after the treatment with filter media, using standard methods. Optimum operating treatment time was determined for maximum removal of these impurities by running the experiment for 2, 4, 6, 8, 10 and 12h, respectively. The maximum reduction of fluoride, arsenic and coliform bacteria in percentage was 85.60%, 93.07% and 100% and their residual values were 0.72 mg/l, 0.009 mg/l and 0 coliform cells/100ml, respectively after a treatment time of 10h. These residual values were under the permissible limits prescribed by WHO. Hence this could be a cheap, easy and an efficient technique for removal of fluoride, arsenic and coliform bacteria from drinking water.

  8. Validation of a QuEChERS-based gas chromatographic method for analysis of pesticide residues in Cassia angustifolia (senna).

    PubMed

    Tripathy, Vandana; Saha, Ajoy; Patel, Dilipkumar J; Basak, B B; Shah, Paresh G; Kumar, Jitendra

    2016-08-02

    A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy-precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01-1.0 μg mL(-1) for OCs and OPs and 0.05-2.5 μg mL(-1) for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70-120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg(-1), and the LOQs were determined as 0.01-0.049 mg kg(-1). The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India.

  9. Kinetics of diuron under aerobic condition and residue analysis in sugarcane under subtropical field conditions.

    PubMed

    Tandon, Shishir; Pant, Ravi

    2017-10-10

    The phenylureas group includes persistent herbicides which are major pollutants to soil and water. Dissipation kinetics of diuron in different soils under sugarcane field conditions was investigated. Diuron was extracted with acetone and florisil solid phase extraction clean-up and characterized by high-performance liquid chromatography-UV. Diuron persisted for more than 100 days and dissipation followed monophasic first-order kinetics. Persistence was more in sandy loam compared to silty clay loam soil. Half-life of diuron in silty clay loam soil was 22.57 and 32.37 days and in sandy loam was 28.35 and 43.93 days at 2 and 4 kg ha-1applications, respectively. Average recovery in soil, bagasse, leaf-straw and juice ranged from 75.95% to 84.20%, 80.15% to 89.35%, 77.46% to 86.19% and 81.88% to 92.68%, respectively. The quantitation limits for soil, bagasse, leaf-straw and juice were 0.01, 0.03, 0.04 μg g -1 and 0.008 μg mL -1 , respectively. Application of diuron inhibited growth of soil microbes initially but they recovered later. At harvest, diuron residues were below maximum residue limits in all samples. The study revealed that under subtropical conditions, diuron is safe for use in weed management and would not pose any residual/environmental problem and that sugarcane crop could be used safe for human/animal consumption.

  10. Dissipation and Residues of Pyrethrins in Leaf Lettuce under Greenhouse and Open Field Conditions.

    PubMed

    Pan, Lixiang; Feng, Xiaoxiao; Zhang, Hongyan

    2017-07-21

    Pyrethrins are nowadays widely used for prevention and control of insects in leaf lettuce. However, there is a concern about the pesticide residue in leaf lettuce. A reliable analytical method for determination of pyrethrins (pyrethrin-and П, cinerin І and П, and jasmolin І and П) in leaf lettuce was developed by using gas chromatography-mass spectrometry (GC-MS). Recoveries of pyrethrins in leaf lettuce at three spiking levels were 99.4-104.0% with relative standard deviations of 0.9-3.1% ( n = 5). Evaluation of dissipation and final residues of pyrethrins in leaf lettuce were determined at six different locations, including the open field, as well as under greenhouse conditions. The initial concentration of pyrethrins in greenhouse (0.57 mg/kg) was higher than in open field (0.25 mg/kg) and the half-life for pyrethrins disappearance in field lettuce (0.7 days) was less than that greenhouse lettuce (1.1 days). Factors such as rainfall, solar radiation, wind speed, and crop growth rate are likely to have caused these results. The final residue in leaf lettuce was far below the maximum residue limits (MRLs) (1 mg/kg established by the European Union (EU), Australia, Korea, Japan).

  11. Multiclass methods for the analysis of antibiotic residues in milk by liquid chromatography coupled to mass spectrometry: A review.

    PubMed

    Rossi, Rosanna; Saluti, Giorgio; Moretti, Simone; Diamanti, Irene; Giusepponi, Danilo; Galarini, Roberta

    2018-02-01

    Milk is an important and beneficial food from a nutritional point of view, being an indispensable source of high quality proteins. Furthermore, it is a raw material for many dairy products, such as yoghurt, cheese, cream etc. Before reaching consumers, milk goes through production, processing and circulation. Each step involves potentially unsafe factors, such as chemical contamination that can affect milk quality. Antibiotics are widely used in veterinary medicine for dry cow therapy and mastitis treatment in lactating cows, which can cause the presence of antimicrobial residues in milk. In order to ensure consumers' safety, milk is analyzed to make sure that the fixed Maximum Residue Limits (MRLs) for antibiotics are not exceeded. Multiclass methods can monitor more drug classes through a single analysis, so they are faster, less time-consuming and cheaper than traditional methods (single-class); this aspect is particularly important for milk, which is a highly perishable food. Nevertheless, multiclass methods for veterinary drug residues in foodstuffs are real analytical challenges. This article reviews the major multiclass methods published for the determination of antibiotic residues in milk by liquid chromatography coupled to mass spectrometry, with a special focus on sample preparation approaches.

  12. Ligand replacement-induced fluorescence switch of quantum dots for ultrasensitive detection of organophosphorothioate pesticides.

    PubMed

    Zhang, Kui; Mei, Qingsong; Guan, Guijian; Liu, Bianhua; Wang, Suhua; Zhang, Zhongping

    2010-11-15

    The development of a simple and on-site assay for the detection of organophosphorus pesticed residues is very important for food safety and exosystem protection. This paper reports the surface coordination-originated fluorescence resonance energy transfer (FRET) of CdTe quantum dots (QDs) and a simple ligand-replacement turn-on mechanism for the highly sensitive and selective detection of organophosphorothioate pesticides. It has been demonstrated that coordination of dithizone at the surface of CdTe QDs in basic media can strongly quench the green emission of CdTe QDs by a FRET mechanism. Upon the addition of organophosphorothioate pesticides, the dithizone ligands at the CdTe QD surface are replaced by the hydrolyzate of the organophosphorothioate, and hence the fluorescence is turned on. The fluorescence turn on is immediate, and the limit of detection for chlorpyrifos is as low as ∼0.1 nM. Two consecutive linear ranges allow a wide determination of chlorpyrifos concentrations from 0.1 nM to 10 μM. Importantly, the fluorescence turn-on chemosensor can directly detect chlorpyrifos residues in apples at a limit of 5.5 ppb, which is under the maximum residue limit allowed by the U.S. Environmental Protection Agency. The very simple strategy reported here should facilitate the development of fluorescence turn-on chemosensors for chemo/biodetection.

  13. Monitoring of pesticide residues in market basket samples of vegetable from Lucknow City, India: QuEChERS method.

    PubMed

    Srivastava, Ashutosh K; Trivedi, Purushottam; Srivastava, M K; Lohani, M; Srivastava, Laxman Prasad

    2011-05-01

    The study was conducted on 20 vegetables including leafy, root, modified stem, and fruity vegetables like bitter gourd, jack fruit, french-bean, onion, colocassia, pointed gourd, capsicum, spinach, potato, fenugreek seeds, carrot, radish, cucumber, beetroot, brinjal, cauliflower, cabbage, tomato, okra, and bottle gourd. Forty-eight pesticides including 13 organochlorines (OCs), 17 organophosphates (OPs), 10 synthetic pyrethriods (SPs), and eight herbicides (H) pesticides were analyzed. A total number of 60 samples, each in triplicates, were analyzed using Quick, Easy, Cheap, Effective, Rugged, and Safe method. The quantification was done by GC-ECD/NPD. The recovery varies from 70.22% to 96.32% with relative standard deviation (RSD) of 15%. However the limit of detection ranged from 0.001-0.009 mg kg(-1)for OCs, SPs, OPs, and H, respectively. Twenty-three pesticides were detected from total 48 analyzed pesticides in the samples with the range of 0.005-12.35 mg kg(-1). The detected pesticides were: Σ-HCH, Dicofol, Σ-Endosulfan, Fenpropathrin, Permethrin-II, β-cyfluthrin-II, Fenvalerate-I, Dichlorvos, Dimethoate, Diazinon, Malathion, Chlorofenvinfos, Anilophos, and Dimethachlor. In some vegetables like radish, cucumber, cauliflower, cabbage, and okra, the detected pesticides (Σ-HCH, Permethrin-II, Dichlorvos, and Chlorofenvinfos) were above maximum residues limit (MRL) (PFA 1954). However, in other vegetables the level of pesticide residues was either below detection limit or MRL.

  14. On the residual stress modeling of shot-peened AISI 4340 steel: finite element and response surface methods

    NASA Astrophysics Data System (ADS)

    Asgari, Ali; Dehestani, Pouya; Poruraminaie, Iman

    2018-02-01

    Shot peening is a well-known process in applying the residual stress on the surface of industrial parts. The induced residual stress improves fatigue life. In this study, the effects of shot peening parameters such as shot diameter, shot speed, friction coefficient, and the number of impacts on the applied residual stress will be evaluated. To assess these parameters effect, firstly the shot peening process has been simulated by finite element method. Then, effects of the process parameters on the residual stress have been evaluated by response surface method as a statistical approach. Finally, a strong model is presented to predict the maximum residual stress induced by shot peening process in AISI 4340 steel. Also, the optimum parameters for the maximum residual stress are achieved. The results indicate that effect of shot diameter on the induced residual stress is increased by increasing the shot speed. Also, enhancing the friction coefficient magnitude always cannot lead to increase in the residual stress.

  15. Characterization of 3-Dimensional PET Systems for Accurate Quantification of Myocardial Blood Flow.

    PubMed

    Renaud, Jennifer M; Yip, Kathy; Guimond, Jean; Trottier, Mikaël; Pibarot, Philippe; Turcotte, Eric; Maguire, Conor; Lalonde, Lucille; Gulenchyn, Karen; Farncombe, Troy; Wisenberg, Gerald; Moody, Jonathan; Lee, Benjamin; Port, Steven C; Turkington, Timothy G; Beanlands, Rob S; deKemp, Robert A

    2017-01-01

    Three-dimensional (3D) mode imaging is the current standard for PET/CT systems. Dynamic imaging for quantification of myocardial blood flow with short-lived tracers, such as 82 Rb-chloride, requires accuracy to be maintained over a wide range of isotope activities and scanner counting rates. We proposed new performance standard measurements to characterize the dynamic range of PET systems for accurate quantitative imaging. 82 Rb or 13 N-ammonia (1,100-3,000 MBq) was injected into the heart wall insert of an anthropomorphic torso phantom. A decaying isotope scan was obtained over 5 half-lives on 9 different 3D PET/CT systems and 1 3D/2-dimensional PET-only system. Dynamic images (28 × 15 s) were reconstructed using iterative algorithms with all corrections enabled. Dynamic range was defined as the maximum activity in the myocardial wall with less than 10% bias, from which corresponding dead-time, counting rates, and/or injected activity limits were established for each scanner. Scatter correction residual bias was estimated as the maximum cavity blood-to-myocardium activity ratio. Image quality was assessed via the coefficient of variation measuring nonuniformity of the left ventricular myocardium activity distribution. Maximum recommended injected activity/body weight, peak dead-time correction factor, counting rates, and residual scatter bias for accurate cardiac myocardial blood flow imaging were 3-14 MBq/kg, 1.5-4.0, 22-64 Mcps singles and 4-14 Mcps prompt coincidence counting rates, and 2%-10% on the investigated scanners. Nonuniformity of the myocardial activity distribution varied from 3% to 16%. Accurate dynamic imaging is possible on the 10 3D PET systems if the maximum injected MBq/kg values are respected to limit peak dead-time losses during the bolus first-pass transit. © 2017 by the Society of Nuclear Medicine and Molecular Imaging.

  16. Evaluation of regulatory variation and theoretical health risk for pesticide maximum residue limits in food.

    PubMed

    Li, Zijian

    2018-08-01

    To evaluate whether pesticide maximum residue limits (MRLs) can protect public health, a deterministic dietary risk assessment of maximum pesticide legal exposure was conducted to convert global MRLs to theoretical maximum dose intake (TMDI) values by estimating the average food intake rate and human body weight for each country. A total of 114 nations (58% of the total nations in the world) and two international organizations, including the European Union (EU) and Codex (WHO) have regulated at least one of the most currently used pesticides in at least one of the most consumed agricultural commodities. In this study, 14 of the most commonly used pesticides and 12 of the most commonly consumed agricultural commodities were identified and selected for analysis. A health risk analysis indicated that nearly 30% of the computed pesticide TMDI values were greater than the acceptable daily intake (ADI) values; however, many nations lack common pesticide MRLs in many commonly consumed foods and other human exposure pathways, such as soil, water, and air were not considered. Normality tests of the TMDI values set indicated that all distributions had a right skewness due to large TMDI clusters at the low end of the distribution, which were caused by some strict pesticide MRLs regulated by the EU (normally a default MRL of 0.01 mg/kg when essential data are missing). The Box-Cox transformation and optimal lambda (λ) were applied to these TMDI distributions, and normality tests of the transformed data set indicated that the power transformed TMDI values of at least eight pesticides presented a normal distribution. It was concluded that unifying strict pesticide MRLs by nations worldwide could significantly skew the distribution of TMDI values to the right, lower the legal exposure to pesticide, and effectively control human health risks. Copyright © 2018 Elsevier Ltd. All rights reserved.

  17. High-Throughput Analytical Techniques for the Determination of the Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea, Part VII: A GC-MS, GC-MS/MS, and LC-MS/MS Study of the Degradation Profiles of Pesticide Residues in Green Tea.

    PubMed

    Chang, Qiao-Ying; Pang, Guo-Fang; Fan, Chun-Lin; Chen, Hui; Yang, Fang; Li, Jie; Wen, Bi-Fang

    2016-11-01

    GC-MS, GC-tandem MS (MS/MS), and LC-MS/MS were used to mathematically define the degradation profiles of pesticide residues in two field trials. Nineteen pesticides were studied in the first field trial and 11 in the second. The results of the field trials demonstrated that the degradation profiles of pesticide residues in green tea can be described with power functions to successfully estimate the amount of time, following pesticide application, pesticide residues appearing in tea in concentrations at and/or above the maximum residue limit (MRL) decrease to concentrations below the MRL. Stability tests on green tea samples stored at room temperature were conducted to determine whether pesticide-incurred green tea samples prepared according to the method used in the field trials would be suitable for the preparation of reference standards for laboratory-proficiency testing trials. This paper reports the results of a GC-MS, GC-MS/MS, and LC-MS/MS study, as well as the suitability of the samples prepared under these conditions for use as pesticide reference standards in tea analysis.

  18. Food safety in Thailand. 3: Pesticide residues detected in mangosteen (Garcinia mangostana L.), queen of fruits.

    PubMed

    Phopin, Kamonrat; Wanwimolruk, Sompon; Prachayasittikul, Virapong

    2017-02-01

    For developing countries like Thailand, regulation of pesticide usage exists, but it is not fully enforced. Therefore, pesticide residues in vegetables and fruits have not been well monitored. This study aimed to determine the pesticide residues in mangosteen fruits sold in Thailand. The mangosteen samples (n = 111) were purchased and the contents of 28 pesticides were analysed by GC-MS/MS method. Of the pesticides tested, eight were found in 100% of the mangosteen samples. However, in 97% of these samples, either chlorothalonil, chlorpyrifos, diazinon, dimethoate, metalaxyl or profenofos was detected exceeding their maximum residue limits (MRLs), representing a 97% rate of pesticide detection above the MRL. This rate is much higher than those found in other fruits sold in developed countries. However, this conclusion excludes the fresh Thai mangosteens grown for export, as these are generally cultivated and harvested to GAP standards. Since the edible part of the mangosteen is the pulp, washing the fruits with running water can reduce the risk of pesticide residues contaminating the pulp which would be eaten by the consumer. The findings strongly suggest that routine monitoring of pesticide residues in fruits and vegetables is required to reduce the health risks associated with consuming contaminated food. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  19. LC/DAD/ESI/MS method for the determination of imidacloprid, thiacloprid, and spinosad in olives and olive oil after field treatment.

    PubMed

    Angioni, Alberto; Porcu, Luciano; Pirisi, Filippo

    2011-10-26

    The behavior in the field and the transfer from olives to olive oil during the technological process of imidacloprid, thiacloprid, and spinosad were studied. The extraction method used was effective in extracting the analytes of interest, and no interfering peaks were detected in the chromatogram. The residue levels found in olives after treatment were 0.14, 0.04, and 0.30 mg/kg for imidacloprid, thiacloprid, and spinosad, respectively, far below the maximum residue levels (MRLs) set for these insecticides in EU. At the preharvest interval (PHI), no residue was detected for imidacloprid and thiacloprid, while spinosad showed a residue level of 0.04 mg/kg. The study of the effect of the technological process on pesticide transfer in olive oil showed that these insecticides tend to remain in the olive cake. The LC/DAD/ESI/MS method showed good performance with adequate recoveries ranging from 80 to 119% and good method limits of quantitation (LOQs) and of determination (LODs). No matrix effect was detected.

  20. Organochlorine insecticide residues are found in surface, irrigated water samples from several districts in Bangladesh.

    PubMed

    Chowdhury, Alamgir Zaman; Islam, Mohammad Nazrul; Moniruzzaman, Mohammed; Gan, Siew Hua; Alam, Md Khorshed

    2013-02-01

    The purpose of this study was to investigate the occurrence and distribution of organochlorines such as aldrin, dieldrin, dichlorodiphenyldichloroethylene (DDE), dichlorodiphenyldichloroethane (DDD), dichlorodiphenyltrichloroethane (DDT), endrin, lindane and heptachlor insecticide residues in irrigated surface water samples collected from 22 districts in Bangladesh. The concentrations of the pesticides were determined using gas chromatography mass spectrophotometry. Water samples from five locations (Feni, Nawabganj, Putia, Burichang and Chatak) were contaminated with DDT; the highest DDT concentration detected was 8.29 μg/L, and its metabolite, DDE, was detected at 4.06 μg/L. Water samples from four other locations (Natore, Sikderpara, Chatak and Rajoir) were contaminated with heptachlor residues, and the highest level detected was 5.24 μg/L, which is the above the maximum contaminant level recommended by the World Health Organisation. A water sample collected from Chatak, Sunamganj, was contaminated with both DDT and heptachlor pesticide residues. None of the water samples were contaminated with aldrin, DDD, dieldrin, endrin or lindane. It is concluded that continuous, long-term monitoring and essential steps to limit the use of the pesticides in Bangladesh are needed.

  1. Assessment of elimination profile of albendazole residues in fish.

    PubMed

    Busatto, Zenaís; de França, Welliton Gonçalves; Cyrino, José Eurico Possebon; Paschoal, Jonas Augusto Rizzato

    2018-01-01

    Few drugs are specifically regulated for aquaculture. Thus this study considered albendazole (ABZ) as a potential drug for use in fish, which, however, is not yet regulated for this application. ABZ is a broad-spectrum anthelmintic approved for farmed ruminants and recently considered for treatment of fish parasites. It is the subject of careful monitoring because of potential residues in animal products. This study evaluated the depletion of ABZ and its main known metabolites: albendazole sulfoxide - ABZSO, albendazole sulfone - ABZSO 2 and albendazole amino sulfone - ABZ-2-NH 2 SO 2 , in the fillets of the Neotropical Characin pacu, Piaractus mesopotamicus, which were fed diets containing 10 mg ABZ kg -1 body weight in a single dose. Fish were euthanised at 8, 12, 24, 48, 72, 96 and 120 hours after medication and the depletion profiles of ABZ, each metabolite and the sum of all marker residues were assessed and evaluated taking into account methodological variations regarding determination of the maximum residue limits adopted by different international regulating agencies for estimation of the withdrawal period (WP). The estimated WPs ranged from 2 to 7 days.

  2. Eco-friendly process combining physical-chemical and biological technics for the fermented dairy products waste pretreatment and reuse.

    PubMed

    Kasmi, Mariam; Hamdi, Moktar; Trabelsi, Ismail

    2017-01-01

    Residual fermented dairy products resulting from process defects or from expired shelf life products are considered as waste. Thus, dairies wastewater treatment plants (WWTP) suffer high input effluents polluting load. In this study, fermented residuals separation from the plant wastewater is proposed. In the aim to meet the municipal WWTP input limits, a pretreatment combining physical-chemical and biological processes was investigated to reduce residual fermented dairy products polluting effect. Yoghurt (Y) and fermented milk products (RL) were considered. Raw samples chemical oxygen demand (COD) values were assessed at 152 and 246 g.L -1 for Y and RL products, respectively. Following the thermal coagulation, maximum removal rates were recorded at 80 °C. Resulting whey stabilization contributed to the removal rates enhance to reach 72% and 87% for Y and RL samples; respectively. Residual whey sugar content was fermented using Candida strains. Bacterial growth and strains degrading potential were discussed. C. krusei strain achieved the most important removal rates of 78% and 85% with Y and RL medium, respectively. Global COD removal rates exceeded 93%.

  3. Residue evaluation of imidacloprid, spirotetramat, and spirotetramat-enol in/on grapes (Vitis vinifera L.) and soil.

    PubMed

    Mohapatra, Soudamini; Kumar, Sampath; Prakash, G S

    2015-10-01

    A combination of imidacloprid and spirotetramat effectively controls sucking pests on grapevines. Residues of these insecticides on grapes were evaluated after treatment with spirotetramat 12% + imidacloprid 12% (240 SC) three times at 90 and 180 g a.i. ha(-1). The samples were extracted and purified by QuEChERS method and analyzed by high-performance liquid chromatography with a photodiode array detector (imidacloprid) and gas chromatography mass spectrometry (spirotetramat and its metabolite spirotetramat-enol). Satisfactory results were obtained with ranges of 80.6-98.6% for the recovery, 3.1-10% for the relative standard deviation range, and 9.8-15.6% for the uncertainty. The limits of detection and quantification were 0.015 μg mL(-1) and 0.05 mg kg(-1), respectively. Initial residue concentrations of imidacloprid after the 90 and 180 g a.i. ha(-1) treatments were 0.912 (half-life 11 days) and 1.681 mg kg(-1) (half-life 12.4 days), respectively. For spirotetramat + spirotetramat-enol, the residue concentrations were 1.337 (half-life 5.6 days) and 2.0 mg kg(-1) (half-life 7.6 days) for the 90 and 180 g a.i. ha(-1) treatments, respectively. Spirotetramat degraded faster than spirotetramat-enol. After treatment at 90 g a.i. ha(-1), the initial residues of both insecticides were within European Union maximum residue limits and a 1-day pre-harvest interval (PHI) was adequate for safe consumption of grapes. After treatment at 180 g a.i. ha(-1), the required PHI was 7 day. Therefore, a PHI of 7 day should be used after treatment with imidacloprid and spirotetramat.

  4. Advanced technique for ultra-thin residue inspection with sub-10nm thickness using high-energy back-scattered electrons

    NASA Astrophysics Data System (ADS)

    Han, Jin-Hee

    2018-03-01

    Recently the aspect ratio of capacitor and via hole of memory semiconductor device has been dramatically increasing in order to store more information in a limited area. A small amount of remained residues after etch process on the bottom of the high aspect ratio structure can make a critical failure in device operation. Back-scattered electrons (BSE) are mainly used for inspecting the defect located at the bottom of the high aspect ratio structure or analyzing the overlay of the multi-layer structure because these electrons have a high linearity with the direction of emission and a high kinetic energy above 50eV. However, there is a limitation on that it cannot detect ultra-thin residue material having a thickness of several nanometers because the surface sensitivity is extremely low. We studied the characteristics of BSE spectra using Monte Carlo simulations for several cases which the high aspect ratio structures have extreme microscopic residues. Based on the assumption that most of the electrons emitted without energy loss are localized on the surface, we selected the detection energy window which has a range of 20eV below the maximum energy of the BSE. This window section is named as the high-energy BSE region. As a result of comparing the detection sensitivity of the conventional and the high-energy BSE detection mode, we found that the detection sensitivity for the residuals which have 2nm thickness is improved by more than 10 times in the high-energy BSE mode. This BSE technology is a new inspection method that can greatly be improved the inspection sensitivity for the ultra-thin residual material presented in the high aspect ratio structure, and its application will be expanded.

  5. Food safety in Thailand 4: comparison of pesticide residues found in three commonly consumed vegetables purchased from local markets and supermarkets in Thailand.

    PubMed

    Wanwimolruk, Sompon; Phopin, Kamonrat; Boonpangrak, Somchai; Prachayasittikul, Virapong

    2016-01-01

    The wide use of pesticides raises concerns on the health risks associated with pesticide exposure. For developing countries, like Thailand, pesticide monitoring program (in vegetables and fruits) and also the maximum residue limits (MRL) regulation have not been entirely implemented. The MRL is a product limit, not a safety limit. The MRL is the maximum concentration of a pesticide residue (expressed as mg/kg) recommended by the Codex Alimentarius Commission to be legally permitted in or on food commodities and animal feeds (Codex Alimentarius Commission, 2015; European Commission, 2015). MRLs are based on supervised residue trial data where the pesticide has been applied in accordance with GAP (Good Agricultural Practice). This study aims at providing comparison data on pesticide residues found in three commonly consumed vegetables (Chinese kale, pakchoi and morning glory) purchased from some local markets and supermarkets in Thailand. These vegetables were randomly bought from local markets and supermarkets. Then they were analyzed for the content of 28 pesticides by using GC-MS/MS. Types of pesticides detected in the samples either from local markets or supermarkets were similar. The incidence of detected pesticides was 100% (local markets) and 99% (supermarkets) for the Chinese kale; 98% (local markets) and 100% (supermarkets) for the pakchoi; and 99% (local markets) and 97% (supermarkets) for the morning glory samples. The pesticides were detected exceeding their MRL at a rate of 48% (local markets) and 35% (supermarkets) for the Chinese kale; 71% (local markets) and 55% (supermarkets) for the pakchoi, and 42% (local markets) and 49% (supermarkets) for the morning glory. These rates are much higher than those seen in developed countries. It should be noted that these findings were assessed on basis of using criteria (such as MRL) obtained from developed countries. Our findings were also confined to these vegetables sold in a few central provinces of Thailand and did not reflect for the whole country as sample sizes were small. Risk assessment due to consuming these pesticide contaminated vegetables, still remains to be evaluated. However, remarkably high incidence rates of detected pesticides give warning to the Thai authorities to implement proper regulations on pesticide monitoring program. Similar incidence of pesticide contamination found in the vegetables bought from local markets and supermarkets raises question regarding the quality of organic vegetables domestically sold in Thailand. This conclusion excludes Thai export quality vegetables and fruits routinely monitored for pesticide contamination before exporting.

  6. Food safety in Thailand 4: comparison of pesticide residues found in three commonly consumed vegetables purchased from local markets and supermarkets in Thailand

    PubMed Central

    Phopin, Kamonrat; Boonpangrak, Somchai; Prachayasittikul, Virapong

    2016-01-01

    Background The wide use of pesticides raises concerns on the health risks associated with pesticide exposure. For developing countries, like Thailand, pesticide monitoring program (in vegetables and fruits) and also the maximum residue limits (MRL) regulation have not been entirely implemented. The MRL is a product limit, not a safety limit. The MRL is the maximum concentration of a pesticide residue (expressed as mg/kg) recommended by the Codex Alimentarius Commission to be legally permitted in or on food commodities and animal feeds (Codex Alimentarius Commission, 2015; European Commission, 2015). MRLs are based on supervised residue trial data where the pesticide has been applied in accordance with GAP (Good Agricultural Practice). This study aims at providing comparison data on pesticide residues found in three commonly consumed vegetables (Chinese kale, pakchoi and morning glory) purchased from some local markets and supermarkets in Thailand. Methods These vegetables were randomly bought from local markets and supermarkets. Then they were analyzed for the content of 28 pesticides by using GC-MS/MS. Results Types of pesticides detected in the samples either from local markets or supermarkets were similar. The incidence of detected pesticides was 100% (local markets) and 99% (supermarkets) for the Chinese kale; 98% (local markets) and 100% (supermarkets) for the pakchoi; and 99% (local markets) and 97% (supermarkets) for the morning glory samples. The pesticides were detected exceeding their MRL at a rate of 48% (local markets) and 35% (supermarkets) for the Chinese kale; 71% (local markets) and 55% (supermarkets) for the pakchoi, and 42% (local markets) and 49% (supermarkets) for the morning glory. Discussion These rates are much higher than those seen in developed countries. It should be noted that these findings were assessed on basis of using criteria (such as MRL) obtained from developed countries. Our findings were also confined to these vegetables sold in a few central provinces of Thailand and did not reflect for the whole country as sample sizes were small. Risk assessment due to consuming these pesticide contaminated vegetables, still remains to be evaluated. However, remarkably high incidence rates of detected pesticides give warning to the Thai authorities to implement proper regulations on pesticide monitoring program. Similar incidence of pesticide contamination found in the vegetables bought from local markets and supermarkets raises question regarding the quality of organic vegetables domestically sold in Thailand. This conclusion excludes Thai export quality vegetables and fruits routinely monitored for pesticide contamination before exporting. PMID:27635366

  7. Predicting protein β-sheet contacts using a maximum entropy-based correlated mutation measure.

    PubMed

    Burkoff, Nikolas S; Várnai, Csilla; Wild, David L

    2013-03-01

    The problem of ab initio protein folding is one of the most difficult in modern computational biology. The prediction of residue contacts within a protein provides a more tractable immediate step. Recently introduced maximum entropy-based correlated mutation measures (CMMs), such as direct information, have been successful in predicting residue contacts. However, most correlated mutation studies focus on proteins that have large good-quality multiple sequence alignments (MSA) because the power of correlated mutation analysis falls as the size of the MSA decreases. However, even with small autogenerated MSAs, maximum entropy-based CMMs contain information. To make use of this information, in this article, we focus not on general residue contacts but contacts between residues in β-sheets. The strong constraints and prior knowledge associated with β-contacts are ideally suited for prediction using a method that incorporates an often noisy CMM. Using contrastive divergence, a statistical machine learning technique, we have calculated a maximum entropy-based CMM. We have integrated this measure with a new probabilistic model for β-contact prediction, which is used to predict both residue- and strand-level contacts. Using our model on a standard non-redundant dataset, we significantly outperform a 2D recurrent neural network architecture, achieving a 5% improvement in true positives at the 5% false-positive rate at the residue level. At the strand level, our approach is competitive with the state-of-the-art single methods achieving precision of 61.0% and recall of 55.4%, while not requiring residue solvent accessibility as an input. http://www2.warwick.ac.uk/fac/sci/systemsbiology/research/software/

  8. The impact of seasonal variation on organochlorine pesticide residues in buffalo and cow milk of selected dairy farms from Faisalabad region.

    PubMed

    Sajid, Muhammad Wasim; Shamoon, Muhammad; Randhawa, Muhammad Atif; Asim, Muhammad; Chaudhry, Abdul Shakoor

    2016-10-01

    Two hundred milk samples from 20 randomly selected dairy farms were screened for the incidence of organochlorine pesticide residues to evaluate the safety of milk in Faisalabad region. The results revealed that overall buffalo milk samples in winter (85 %) and in summer (78 %) were more contaminated as compared to cow milk samples 83 and 75 % in respective seasons. The residues of cyhalothrin were found only in summer season in milk of both species. Permethrin residues were detected at higher levels than perfinofos while DDT and methamedophos were found undetectable. The mean levels of permethrin were 0.042 and 0.033 mg kg -1 in buffalo milk samples and 0.045 and 0.043 mg kg -1 in cow milk in winter and summer season, respectively. Perfinofos residues were found to be the least contaminated pesticides with mean values of 0.0006 and 0.0013 mg kg -1 , respectively in winter season, and 0.004 and 0.0025 mg kg -1 in summer season. All analysed pesticide residues in milk samples in both seasons were below the maximum residual limit (MRL) values as described by European Union (EU) but milk samples contaminated with α, β-endosulfan and endosulphate exceeded their respective Food and Agriculture Organization's (FAO) established MRLs both in winter and summer.

  9. Long-lived radionuclides in residues from operation and decommissioning of nuclear power plants

    NASA Astrophysics Data System (ADS)

    López-Gutiérrez, J. M.; Gómez-Guzmán, J. M.; Chamizo, E.; Peruchena, J. I.; García-León, M.

    2013-01-01

    Radioactive residues, in order to be classified as Low-Level Waste (LLW), need to fulfil certain conditions; the limitation of the maximum activity from long-lived radionuclides is one of these requirements. In order to verify compliance to this limitation, the abundance of these radionuclides in the residue must be determined. However, performing this determination through radiometric methods constitutes a laborious task. In this work, 129I concentrations, 239+240Pu activities, and 240Pu/239Pu ratios are determined in low-level radioactive residues, including resins and dry sludge, from nuclear power plants in Spain. The use of Accelerator Mass Spectrometry (AMS) enables high sensitivities to be achieved, and hence these magnitudes can be re determined with good precision. Results present a high dispersion between the 129I and 239+240Pu activities found in various aliquots of the same sample, which suggests the existence of a mixture of resins with a variety of histories in the same container. As a conclusion, it is shown that activities and isotopic ratios can provide information on the processes that occur in power plants throughout the history of the residues. Furthermore, wipes from the monitoring of surface contamination of the José Cabrera decommissioning process have been analyzed for 129I determination. The wide range of measured activities indicates an effective dispersal of 129I throughout the various locations within a nuclear power plant. Not only could these measurements be employed in the contamination monitoring of the decommissioning process, but also in the modelling of the presence of other iodine isotopes.

  10. 40 CFR 141.66 - Maximum contaminant levels for radionuclides.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 24 2012-07-01 2012-07-01 false Maximum contaminant levels for... Regulations: Maximum Contaminant Levels and Maximum Residual Disinfectant Levels § 141.66 Maximum contaminant levels for radionuclides. (a) [Reserved] (b) MCL for combined radium-226 and -228. The maximum...

  11. 40 CFR 141.66 - Maximum contaminant levels for radionuclides.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 23 2014-07-01 2014-07-01 false Maximum contaminant levels for... Regulations: Maximum Contaminant Levels and Maximum Residual Disinfectant Levels § 141.66 Maximum contaminant levels for radionuclides. (a) [Reserved] (b) MCL for combined radium-226 and -228. The maximum...

  12. 40 CFR 141.66 - Maximum contaminant levels for radionuclides.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 24 2013-07-01 2013-07-01 false Maximum contaminant levels for... Regulations: Maximum Contaminant Levels and Maximum Residual Disinfectant Levels § 141.66 Maximum contaminant levels for radionuclides. (a) [Reserved] (b) MCL for combined radium-226 and -228. The maximum...

  13. 40 CFR 141.66 - Maximum contaminant levels for radionuclides.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 23 2011-07-01 2011-07-01 false Maximum contaminant levels for... Regulations: Maximum Contaminant Levels and Maximum Residual Disinfectant Levels § 141.66 Maximum contaminant levels for radionuclides. (a) [Reserved] (b) MCL for combined radium-226 and -228. The maximum...

  14. Emission of Carbon Dioxide Influenced by Different Water Levels from Soil Incubated Organic Residues

    PubMed Central

    Hossain, M. B.; Puteh, A. B.

    2013-01-01

    We studied the influence of different organic residues and water levels on decomposition rate and carbon sequestration in soil. Organic residues (rice straw, rice root, cow dung, and poultry litter) including control were tested under moistened and flooding systems. An experiment was laid out as a complete randomized design at 25°C for 120 days. Higher CO2-C (265.45 mg) emission was observed in moistened condition than in flooding condition from 7 to 120 days. Among the organic residues, poultry litter produced the highest CO2-C emission. Poultry litter with soil mixture increased 121% cumulative CO2-C compared to control. On average, about 38% of added poultry litter C was mineralized to CO2-C. Maximum CO2-C was found in 7 days after incubation and thereafter CO2-C emission was decreased with the increase of time. Control produced the lowest CO2-C (158.23 mg). Poultry litter produced maximum cumulative CO2-C (349.91 mg). Maximum organic carbon was obtained in cow dung which followed by other organic residues. Organic residues along with flooding condition decreased cumulative CO2-C, k value and increased organic C in soil. Maximum k value was found in poultry litter and control. Incorpored rice straw increased organic carbon and decreased k value (0.003 g d−1) in soil. In conclusion, rice straw and poultry litter were suitable for improving soil carbon. PMID:24163626

  15. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 7 Agriculture 2 2011-01-01 2011-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed as...

  16. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 7 Agriculture 2 2013-01-01 2013-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed as...

  17. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 7 Agriculture 2 2014-01-01 2014-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed as...

  18. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 7 Agriculture 2 2012-01-01 2012-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed as...

  19. 7 CFR 29.427 - Pesticide residue standards.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Pesticide residue standards. 29.427 Section 29.427... REGULATIONS TOBACCO INSPECTION Regulations Miscellaneous § 29.427 Pesticide residue standards. The maximum concentration of residues of the following pesticides allowed in flue-cured or burley tobacco, expressed as...

  20. Optimization of manganese peroxidase production from Schizophyllum sp. F17 in solid-state fermentation of agro-industrial residues.

    PubMed

    Zhou, Yue; Yang, Bing; Yang, Yang; Jia, Rong

    2014-03-01

    Manganese peroxidase (MnP), a crucial enzyme in lignin degradation, has wide potential applications in environmental protection. However, large-scale industrial application of this enzyme is limited due to several factors primarily related to cost and availability. Special attention has been paid to the production of MnP from inexpensive sources, such as lignocellulosic residues, using solid-state fermentation (SSF) systems. In the present study, a suitable SSF medium for the production of MnP by Schizophyllum sp. F17 from agro-industrial residues has been optimized. The mixed solid medium, comprising pine sawdust, rice straw, and soybean powder at a ratio of 0.52:0.15:0.33, conferred a maximum enzyme activity of 11.18 U/g on the sixth day of SSF. The results show that the use of wastes such as pine sawdust and rice straw makes the enzyme production more economical as well as helps solve environmental problems.

  1. Occurrence and Residue Pattern of Phthalate Esters in Fresh Tea Leaves and during Tea Manufacturing and Brewing.

    PubMed

    Liu, Pingxiang; Chen, Hongping; Gao, Guanwei; Hao, Zhenxia; Wang, Chen; Ma, Guicen; Chai, Yunfeng; Zhang, Lin; Liu, Xin

    2016-11-23

    The residues of 16 phthalate esters (PAEs) in fresh tea leaves and made tea were determined via gas chromatography-tandem mass spectrometry to study their distribution and degradation characteristics during tea planting and processing. Five PAEs were detected in all fresh tea leaves, and higher concentrations were detected in mature leaves. The distribution of PAEs in fresh tea leaves ranged from 69.7 to 2244.0 μg/kg. The degradative percentages of ∑ 5 PAEs during green tea manufacturing ranged from 61 to 63% and were significantly influenced by the drying process. The transfer rates of PAEs-D 4 ranged from 5.2 to 100.6%. PAEs with a high water solubility showed the highest transfer coefficient in the range of 91.8-100.6%, whereas PAEs with a high log K ow showed a low leaching efficiency below 11.9%. These results benefit the risk evaluation and establishment of a maximum residue limit for PAEs in tea.

  2. Multiresidue analysis of 22 sulfonamides and their metabolites in animal tissues using quick, easy, cheap, effective, rugged, and safe extraction and high resolution mass spectrometry (hybrid linear ion trap-Orbitrap).

    PubMed

    Abdallah, H; Arnaudguilhem, C; Jaber, F; Lobinski, R

    2014-08-15

    A new high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) method was developed for a simultaneous multi-residue analysis of 22 sulfonamides (SAs) and their metabolites in edible animal (pig, beef, sheep and chicken) tissues. Sample preparation was optimized on the basis of the "QuEChERS" protocol. The analytes were identified using their LC retention times and accurate mass; the identification was further confirmed by multi-stage high mass accuracy (<5ppm) mass spectrometry. The performance of the method was evaluated according to the EU guidelines for the validation of screening methods for the analysis of veterinary drugs residues. Acceptable values were obtained for: linearity (R(2)<0.99), limit of detection (LOD, 3-26μg/kg), limit of quantification (LOQ, 11-88μg/kg), accuracy (recovery 88-112%), intra- and inter-day precision 1-14 and 1-17%, respectively, decision limit (CCα) and detection capability (CCβ) around the maximum residue limits (MRL) of SAs (100μg/kg). The method was validated by analysis of a reference material FAPAS-02188 "Pig kidney" with ǀ Z-scoreǀ<0.63. The method was applied to various matrices (kidney, liver, muscle) originated from pig, beef, sheep, and chicken) allowing the simultaneous quantification of target sulfonamides at concentration levels above the MRL/2 and the identification of untargeted compounds such as N(4)-acetyl metabolites using multi-stage high mass accuracy mass spectrometry. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Vibration activity evaluation of double-span rotor at rundown caused by its initial curvature and residual unbalance

    NASA Astrophysics Data System (ADS)

    Kostyuk, A. G.; Volokhovskaya, O. A.

    2017-01-01

    The work is dedicated to the study of vibration activity of double-span rotor of turbine unit (TU) consisting of a high-pressure rotor and a rotor of medium-low pressure rotor combined with it (HPR—MLPR system) at the lowest critical rotational frequencies at rundown. When using the design model of the system, it was assumed that the rotors were installed on anisotropic elastic-damper supports, tied among themselves by a rigid clutch, and having the initial curvature (nonremovable initial deflection) and the residual unbalances in both spans. Two types of bearings were considered-elliptical and six-shoe segmental bearings. It was believed that the initial deflection during operation or as a result of noncompliance of start-up conditions initially gets only HPR and the axis shape of unloaded HPR is known and it is a flat curve. The resultant curve of nonremovable deflection of the HPR-MLPR system occurring after installing the shafting into the bearings was also considered flat and located in the same plane as the initial deflection of HPR. The cases of additional presence with the rotors of concentrated residual unbalances in the middle of each span are considered. The case of availability with both rotors of the shafting antisymmetric point unbalances on each of the spans was not considered in this work. The values of each of the factors of vibration activity (of the initial deflection of HPR and residual unbalances of both rotors) were chosen to be equal to the maximum permissible established by the active in the practice of TU operation limitations on the maximum values of the initial deflection of thermally unstable rotor and its residual unbalances. The influence of location of residual unbalances in relation to the initial deflection curve of HPR-MLPR system on the total amplitudes of transient vibrations caused by both excitation factors in the reference points of the system at TU rundown was investigated. It was established that, at the unfavorable relations between directions of curvature of the rotors of HPR-MLPR system and their residual unbalances with segmental bearings, touching in the diaphragm seals in the middle of HPR span is possible.

  4. 40 CFR 141.55 - Maximum contaminant level goals for radionuclides.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Maximum contaminant level goals for... PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Maximum Contaminant Level Goals and Maximum Residual Disinfectant Level Goals § 141.55 Maximum contaminant level goals for radionuclides...

  5. 40 CFR 141.55 - Maximum contaminant level goals for radionuclides.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 23 2011-07-01 2011-07-01 false Maximum contaminant level goals for... PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Maximum Contaminant Level Goals and Maximum Residual Disinfectant Level Goals § 141.55 Maximum contaminant level goals for radionuclides...

  6. Evaluation of an immunobiosensor for the on-site testing of veterinary drug residues at an abattoir. Screening for sulfamethazine in pigs.

    PubMed

    Baxter, G A; O'Connor, M C; Haughey, S A; Crooks, S R; Elliott, C T

    1999-09-01

    A study was conducted to determine the feasibility of performing "on-site" screening for sulfamethazine (SMT), at an abattoir, using a rapid immunobiosensor method. This involved transfer of the biosensor technology and an assay developed in the laboratory, to the cold, humid conditions of a modern pig-processing factory. A pre-determined threshold limit of 0.4 microgram ml-1 SMT in bile was used to identify the likelihood that corresponding tissue samples contained SMT concentrations in excess of the European maximum permissible residue limit of 0.1 mg kg-1. Bile samples containing SMT concentrations above the threshold limit were deemed positive and the corresponding kidney and muscle samples were sent to the laboratory for HPLC analysis. The robustness of the biosensor instrumentation in the harsh operating conditions was monitored throughout the project. The performance of the assay, on-site, was assessed by the regular inclusion of QA samples and by the submission of control 'SMT-positive' pigs to the abattoir. Sampling procedures, identification and traceability were also under scrutiny. During the project, 337 (9.35%) of the total kill were tested for SMT residues, representing 75% of all producers submitting pigs for slaughter. Twelve animals, including the ten controls, gave positive bile results. HPLC analysis confirmed SMT residues in all 12 kidneys (11 in excess of the permissible level). Ten muscle samples also contained violative SMT levels. Throughout the project, the biosensor performed reliably, with no adverse reaction of any mechanical or electrical components. The SMT assay also performed reliably. This is the first report of a biosensor being used for 'on-site' drug screening.

  7. Residue analysis of tetracyclines in poultry muscle: shortcomings revealed by a proficiency test.

    PubMed

    Berendsen, B J A; Van Rhijn, J A

    2006-11-01

    A proficiency test for tetracycline drug residues in poultry muscle was organized according to the guidelines of International Laboratory Accreditation Cooperation (ILAC) ILAC-G13:2000 (2000). For the proficiency test, three test materials were prepared. The homogeneity and stability of the materials during the study were demonstrated. Sixteen laboratories accepted the invitation to participate in the proficiency test; 11 laboratories reported results within the time frame of the study. Most notably, only four of the participating laboratories complied with the definition of the maximum residue limit (MRL) concerning the inclusion of 4-epimers as stated in European Commission Regulation 281/96 (1996). Most participants reported values for the decision limit (CCalpha) and detection capability (CCbeta) and hence were already in compliance with European Commission 2002/657/EC (2002) for this aspect of method validation. However, some CCalpha and CCbeta values were not in agreement with the actual within-laboratory reproducibility calculated from the results reported in this proficiency test. Although most laboratories obtained satisfactory results, it is clear that an effort is needed to include 4-epiOTC, 4-epiTC and 4-epiCTC in the analytical methods. Moreover, reconsideration of values determined for CCalpha and CCbeta with respect to their accuracy may be necessary in some cases.

  8. Dynamic residual pattern of azoxystrobin in Swiss chard with contribution to safety evaluation.

    PubMed

    Farha, Waziha; Abd El-Aty, A M; Rahman, Md Musfiqur; Kabir, Md Humayun; Chung, Hyung Suk; Lee, Han Sol; Jeon, Jong-Sup; Wang, Jing; Chang, Byung-Joon; Shin, Ho-Chul; Shim, Jae-Han

    2018-02-01

    This study aimed at quantifying the residual amount of azoxystrobin in Swiss chard samples grown under greenhouse conditions at two different locations (Gwangju and Naju, Republic of Korea). Samples were extracted with acetonitrile, separated by salting out, and subjected to purification by using solid-phase extraction. The analyte was identified using liquid chromatography-ultraviolet detection. The linearity of the calibration range was excellent with coefficient of determination 1.00. Recovery at three different spiking levels (0.1, 0.5, and 4 mg/kg) ranged between 82.89 and 109.46% with relative standard deviation <3. The limit of quantification, 0.01 mg/kg, was considerably much lower than the maximum residue limit (50 mg/kg) set by the Korean Ministry of Food and Drug Safety. The developed methodology was successfully used for field-treated leaves, which were collected randomly at 0-14 days following azoxystrobin application. The rate of disappearance in/on Swiss chard was ascribed to first-order kinetics with a half-life of 8 and 5 days, in leaves grown in Gwangju and Naju greenhouses, respectively. Risk assessments revealed that the acceptable daily intake percentage is substantially below the risk level of consumption at day 0 (in both areas), thus encouraging its safe consumption. Copyright © 2017 John Wiley & Sons, Ltd.

  9. Simultaneous determination of sulfonamides, penicillins and coccidiostats in pork by high-performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Nebot, C; Regal, P; Miranda, J; Cepeda, A; Fente, C

    2012-05-01

    Veterinary drugs are widely and legally used to treat and prevent disease in livestock. However, drugs are also used illegally as growth-promoting agents. To protect the health of consumers, maximum residue limits (MRL) in food of animal origin have been established and are listed in Regulation 37/2010. According to this regulation, more than 300 drugs need to be controlled regularly in laboratories for residues of veterinary drugs. A cost-effective analytical method is very important and explains why the development of multi-residual methods is becoming popular in laboratories. The aim of this work is to describe a simple, rapid and economical high-performance liquid chromatography-tandem mass spectrometry method for the simultaneous identification and quantification of 21 veterinary drugs in pork muscle samples. The sample clean-up procedure is performed with acidified dichloromethane and does not require solid phase extraction. The method is applicable to nine sulfonamides and seven coccidiostats identified within 36 min. Calculated relevant validation parameters such as recoveries (from 72.to 126 %), intra-precision and intermediate precision (relative standard deviation below 40 %) and decision limits (below 7 µg Kg(-1)) were within acceptable range and in compliance with the requirements of Commission Decision 2002/657/EC. © The Author [2012]. Published by Oxford University Press. All rights reserved.

  10. Simple and sensitive monitoring of β2-agonist residues in meat by liquid chromatography-tandem mass spectrometry using a QuEChERS with preconcentration as the sample treatment.

    PubMed

    Xiong, Lin; Gao, Ya-Qin; Li, Wei-Hong; Yang, Xiao-Lin; Shimo, Shimo Peter

    2015-07-01

    A liquid chromatography with tandem mass spectrometric detection (LC-MS/MS) method was established for the simultaneous determination of the levels of 10 β2-agonists in meat. The samples were extracted using an aqueous acidic solution and cleaned up using a Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) technique utilising a DVB-NVP-SO3Na sorbent synthesised in-house. First, the β2-agonist residues were extracted in an aqueous acidic solution, followed by matrix solid-phase dispersion for clean-up. The linearities of the method were R(2)=0.9925-0.9998, with RSDs of 2.7-15.3% and 73.7-103.5% recoveries. Very low limits of detection (LOD) and quantitation (LOQ) of 0.2-0.9 μg/kg and 0.8-3.2 μg/kg, respectively, were achieved for spiked meat. The values obtained were lower than the maximum residue limits (MRLs) established by the EU and China. These results clearly demonstrate the feasibility of the proposed approach. The evaluated method provided reliable screening, quantification and identification of 10 β2-agonists in meat. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Distribution of cadmium in leg muscle and liver of game birds from Serbia

    NASA Astrophysics Data System (ADS)

    Nikolić, D.; Đinović-Stojanović, J.; Stefanović, S.; Radičević, T.; Trbović, D.; Spirić, D.; Janković, S.

    2017-09-01

    The aim of this study was to present the distribution of cadmium (Cd) levels in leg muscle and liver of game birds. Samples (n=464) of: pheasants (n=182), mallards (n=25), Eurasian jay (n=7), partridges (n=5), woodcocks (n=8) and common quail (n=5) were collected during regular hunting seasons within the Serbian National Residue Monitoring Program from 2013 to 2016. Analysis of Cd was performed by ICP-MS. In all liver samples, Cd levels were above the limit of detection (LOD=0.001 mg/kg) while in 66.4% of muscle samples, Cd was detected. Statistical analysis showed significant differences between Cd levels in leg muscle and liver of woodcocks and others game birds. The highest mean Cd level was observed in muscle samples of woodcocks (0.042 mg/kg). The lowest mean Cd levels in liver were observed in common quails (0.130 mg/kg) and mallards (0.160 mg/kg) while the highest levels were measured in woodcocks (1.247 mg/kg) and pheasants (0.262 mg/kg). During four years of the Serbian National Residue Monitoring Program, leg muscle samples of woodcocks (n=3), liver samples of pheasants (n=23), woodcocks (n=6) and mallards (n=3) exceeded the maximum residue limit (MRL).

  12. Foliar Desiccators Glyphosate, Carfentrazone, and Paraquat Affect the Technological and Chemical Properties of Cowpea Grains.

    PubMed

    Lindemann, Igor da Silva; Lang, Gustavo Heinrich; Hoffmann, Jessica Fernanda; Rombaldi, Cesar Valmor; de Oliveira, Maurício; Elias, Moacir Cardoso; Vanier, Nathan Levien

    2017-08-16

    The effects of the use of glyphosate (GLY), glyphosate plus carfentrazone (GLY/CAR), and paraquat (PAR) as plant desiccators on the technological and chemical properties of cowpea grains were investigated. All studied desiccants provided lower cooking time to freshly harvested cowpea. However, the coat color of PAR- and GLY/CAR-treated cowpea was reddish in comparison to the control treatment. Principal component analysis (PCA) from liquid chromatography-mass spectrometry (LC-MS) data sets showed a clear distinction among cowpea from the different treatments. Catechin-3-glucoside and epicatechin significantly contributed for discriminating GLY-treated cowpea, while citric acid was responsible for discriminating GLY/CAR-treated cowpea. Quercetin derivative and gluconic acid were responsible for discriminating control treatment. Residual glyphosate and paraquat content was higher than the maximum limits allowed by Codex Alimentarius and the European Union Commission. Improvements in the technological and chemical properties of cowpea may not be overlapped by the risks that those desiccants exhibit when exceeding the maximum limits of tolerance in food.

  13. Occurrence of ivermectin in bovine milk from the Brazilian retail market.

    PubMed

    Lobato, V; Rath, S; Reyes, F G R

    2006-07-01

    High-performance liquid chromatography (HPLC) with fluorescence detection was used for the quantification of ivermectin residues in bovine milk intended for human consumption. After liquid-liquid extraction of ivermectin and purification of the extract, the compound was derivatized with 1-methylimidazol in N,N-dimethyl formamide to form a fluorescent derivative, which was separated by HPLC, using reversed-phase C18, with methanol : water (96 : 4 v/v) mobile phase at a flow rate 0.7 ml min-1. The excitation and emission wavelengths of the fluorescence detector were adjusted at 360 and 470 nm, respectively. The linearity of the method was in the range 10-100 ng ivermectin ml-1. Based on a sample of 5.0 ml, the limit of detection and the limit of quantification for ivermectin in milk were 0.6 and 2 ng ml-1, respectively. The recovery rate varied from 76.4 to 87.2%, with an average of 77.9 +/- 3.2%, at four fortification levels. The inter-day precision of the method was 13% (n = 5). Of 168 samples analysed, 17.8% contained ivermectin above the limit of quantification. Nevertheless, none of the samples contained ivermectin above the maximum residue limit (10 ng ml-1) established by the Brazilian Ministry of Agriculture.

  14. Response of ginger growth to a tetracycline-contaminated environment and residues of antibiotic and antibiotic resistance genes.

    PubMed

    Liu, Xiaohui; Lv, Yao; Xu, Kun; Xiao, Xinxin; Xi, Beidou; Lu, Shaoyong

    2018-06-01

    The presence of antibiotic residues in vegetables has been highlighted as a risk to human health; antibiotics not only cause toxic effects to plants but can also induce antibiotic resistance gene (ARG) expression. Using a soil-free approach, this study aimed to explore the response of ginger growth to tetracycline (TC) pollution and to assess the levels of antibiotic residues in different plant organs and the presence of ARGs in the rhizome. Ginger growth in a highly TC-contaminated environment was remarkably inhibited. Photosynthetic parameters, fluorescence parameters, and some physiological indicators (oxidative substances, photosynthetic pigments, enzyme activity, etc.) were negatively influenced by TC contamination. Although the superoxide dismutase (SOD), peroxidase (POD), and catalase (CAT) activity levels significantly increased, their effects appear to be limited. The accumulation of TC in the rhizome (28.1 mg kg -1 ) was greater than that in the roots, stem, or leaves. All tested antibiotic resistance genes except for tetL were detectable in the rhizome, and their relative abundance was in the order integron1>tetG > tetA > tetC > tetB > tetM. The level of TC in ginger rhizomes was much higher than the maximum residue limits. The potential dose of TC acquired from the consumption of ginger grown in a highly TC-contaminated environment poses no obvious risk to adults but may be a threat to children. Copyright © 2018 Elsevier Ltd. All rights reserved.

  15. Dissipation pattern and risk quotients assessment of amisulbrom in Korean melon cultivated in plastic house conditions.

    PubMed

    Kabir, Md Humayun; Abd El-Aty, A M; Rahman, Md Musfiqur; Chung, Hyung Suk; Lee, Han Sol; Park, Sun-Hyang; Hacımüftüoğlu, Fazil; Chang, Byung-Joon; Shin, Ho-Chul; Shim, Jae-Han

    2017-06-01

    Amisulbrom formulated as suspension concentrate was applied at the rate recommended for Korean melon to determine the dissipation pattern (at two different sites), the pre-harvest residue limit (PHRL), and risk assessments. Samples collected over 10 days were extracted using liquid-liquid extraction (LLE) and cleaned up with solid-phase extraction (SPE) Florisil cartridge. Residual concentrations were determined using liquid chromatography-ultraviolet detector (LC-UVD) and confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The standard showed good instrument response linearity with a correlation coefficient (R 2 ) = 0.9999, and the recovery ranged from 87.5 to 93.7%. The dissipation half-life calculated from two different sites were found to be 7.0 and 8.8 days for sites 1 and 2, respectively. A PHRL graph constructed from the data indicated that if the residue levels were less than 0.55-0.59 mg/kg 3 days before harvest or less than 0.61-0.74 mg/kg 7 days before harvest, then they would be lower than the maximum residue limits (MRLs) at harvest. Risk assessments showed that the risk quotient (RQ) was 4.39-3.47% at 0 day, declined to 1.53-1.63% at 10 days. Therefore, the current data indicate that the amisulbrom can be applied safely to Korean melon; hence, it is unlikely to induce adverse health effects in consumers.

  16. A new molecular evolution model for limited insertion independent of substitution.

    PubMed

    Lèbre, Sophie; Michel, Christian J

    2013-10-01

    We recently introduced a new molecular evolution model called the IDIS model for Insertion Deletion Independent of Substitution [13,14]. In the IDIS model, the three independent processes of substitution, insertion and deletion of residues have constant rates. In order to control the genome expansion during evolution, we generalize here the IDIS model by introducing an insertion rate which decreases when the sequence grows and tends to 0 for a maximum sequence length nmax. This new model, called LIIS for Limited Insertion Independent of Substitution, defines a matrix differential equation satisfied by a vector P(t) describing the sequence content in each residue at evolution time t. An analytical solution is obtained for any diagonalizable substitution matrix M. Thus, the LIIS model gives an expression of the sequence content vector P(t) in each residue under evolution time t as a function of the eigenvalues and the eigenvectors of matrix M, the residue insertion rate vector R, the total insertion rate r, the initial and maximum sequence lengths n0 and nmax, respectively, and the sequence content vector P(t0) at initial time t0. The derivation of the analytical solution is much more technical, compared to the IDIS model, as it involves Gauss hypergeometric functions. Several propositions of the LIIS model are derived: proof that the IDIS model is a particular case of the LIIS model when the maximum sequence length nmax tends to infinity, fixed point, time scale, time step and time inversion. Using a relation between the sequence length l and the evolution time t, an expression of the LIIS model as a function of the sequence length l=n(t) is obtained. Formulas for 'insertion only', i.e. when the substitution rates are all equal to 0, are derived at evolution time t and sequence length l. Analytical solutions of the LIIS model are explicitly derived, as a function of either evolution time t or sequence length l, for two classical substitution matrices: the 3-parameter symmetric substitution matrix [12] (LIIS-SYM3) and the HKY asymmetric substitution matrix[9] (LIIS-HKY). An evaluation of the LIIS model (precisely, LIIS-HKY) based on four statistical analyses of the GC content in complete genomes of four prokaryotic taxonomic groups, namely Chlamydiae, Crenarchaeota, Spirochaetes and Thermotogae, shows the expected improvement from the theory of the LIIS model compared to the IDIS model. Copyright © 2013 Elsevier Inc. All rights reserved.

  17. What is the best method to fit time-resolved data? A comparison of the residual minimization and the maximum likelihood techniques as applied to experimental time-correlated, single-photon counting data

    DOE PAGES

    Santra, Kalyan; Zhan, Jinchun; Song, Xueyu; ...

    2016-02-10

    The need for measuring fluorescence lifetimes of species in subdiffraction-limited volumes in, for example, stimulated emission depletion (STED) microscopy, entails the dual challenge of probing a small number of fluorophores and fitting the concomitant sparse data set to the appropriate excited-state decay function. This need has stimulated a further investigation into the relative merits of two fitting techniques commonly referred to as “residual minimization” (RM) and “maximum likelihood” (ML). Fluorescence decays of the well-characterized standard, rose bengal in methanol at room temperature (530 ± 10 ps), were acquired in a set of five experiments in which the total number ofmore » “photon counts” was approximately 20, 200, 1000, 3000, and 6000 and there were about 2–200 counts at the maxima of the respective decays. Each set of experiments was repeated 50 times to generate the appropriate statistics. Each of the 250 data sets was analyzed by ML and two different RM methods (differing in the weighting of residuals) using in-house routines and compared with a frequently used commercial RM routine. Convolution with a real instrument response function was always included in the fitting. While RM using Pearson’s weighting of residuals can recover the correct mean result with a total number of counts of 1000 or more, ML distinguishes itself by yielding, in all cases, the same mean lifetime within 2% of the accepted value. For 200 total counts and greater, ML always provides a standard deviation of <10% of the mean lifetime, and even at 20 total counts there is only 20% error in the mean lifetime. Here, the robustness of ML advocates its use for sparse data sets such as those acquired in some subdiffraction-limited microscopies, such as STED, and, more importantly, provides greater motivation for exploiting the time-resolved capacities of this technique to acquire and analyze fluorescence lifetime data.« less

  18. High-performance thin-layer chromatography screening of multi class antibiotics in animal food by bioluminescent bioautography and electrospray ionization mass spectrometry.

    PubMed

    Chen, Yisheng; Schwack, Wolfgang

    2014-08-22

    The world-wide usage and partly abuse of veterinary antibiotics resulted in a pressing need to control residues in animal-derived foods. Large-scale screening for residues of antibiotics is typically performed by microbial agar diffusion tests. This work employing high-performance thin-layer chromatography (HPTLC) combined with bioautography and electrospray ionization mass spectrometry introduces a rapid and efficient method for a multi-class screening of antibiotic residues. The viability of the bioluminescent bacterium Aliivibrio fischeri to the studied antibiotics (16 species of 5 groups) was optimized on amino plates, enabling detection sensitivity down to the strictest maximum residue limits. The HPTLC method was developed not to separate the individual antibiotics, but for cleanup of sample extracts. The studied antibiotics either remained at the start zones (tetracyclines, aminoglycosides, fluoroquinolones, and macrolides) or migrated into the front (amphenicols), while interfering co-extracted matrix compounds were dispersed at hRf 20-80. Only after a few hours, the multi-sample plate image clearly revealed the presence or absence of antibiotic residues. Moreover, molecular information as to the suspected findings was rapidly achieved by HPTLC-mass spectrometry. Showing remarkable sensitivity and matrix-tolerance, the established method was successfully applied to milk and kidney samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Abusive use of antibiotics in poultry farming in Cameroon and the public health implications.

    PubMed

    Guetiya Wadoum, R E; Zambou, N F; Anyangwe, F F; Njimou, J R; Coman, M M; Verdenelli, M C; Cecchini, C; Silvi, S; Orpianesi, C; Cresci, A; Colizzi, V

    2016-08-01

    The types and methods of use of antibiotics in poultry farms in Cameroon, residual levels and potential microbial resistance were determined. A questionnaire-based survey identified the different antibiotics used and high-performance liquid chromatography (HPLC) was used to determine residual levels of antibiotics. Pathogens were isolated, identified by use of commercial API kits and minimum inhibition concentration (MIC) was determined. Oxytetracyclin, tylocip and TCN (oxytetracycline, chloramphenicol and neomycin) were the most frequently used antibiotics. Antibiotics screened by HPLC were chloramphenicol, tetracycline and vancomycin. All of them except vancomycin were detected, and the concentration of these antibiotics was higher than the maximum residual limits (MRL) set by regulatory authorities. No residues of various antibiotics were found in egg albumen or yolk. The concentration of tetracycline was significantly higher in liver (150 ± 30 µg/g) than in other tissues. Foodborne pathogens, including Salmonella spp., Staphylococcus spp., Listeria spp., Clostridium spp. and Escherichia spp., were identified. Most of the pathogens were resistant to these various antibiotics tested. These findings imply the need for better management of antibiotic use to control sources of food contamination and reduce health risks associated with the presence of residues and the development of resistant pathogens by further legislation and enforcement of regulations on food hygiene and use of antibiotics.

  20. Development of an enzyme-linked immunosorbent assay for residue analysis of the insecticide emamectin benzoate in agricultural products.

    PubMed

    Kondo, Mika; Yamashita, Hiroshi; Uchigashima, Mikiko; Kono, Takeshi; Takemoto, Toshihide; Fujita, Masahiro; Saka, Machiko; Iwasa, Seiji; Ito, Shigekazu; Miyake, Shiro

    2009-01-28

    A direct competitive enzyme-linked immunosorbent assay (dc-ELISA) for the analysis of emamectin residues in agricultural products was developed using a prepared mouse monoclonal antibody. The working range was 0.3-3.0 ng/mL, and the 50% inhibition concentration (IC(50)) was 1.0 ng/mL. The assay was sufficiently sensitive for analysis of the maximum residue limits in agricultural products in Japan (>0.1 microg/g). Emamectin residues contain the following metabolites: the 4''-epi-amino analogue, the 4''-epi-(N-formyl)amino analogue, the 4''-epi-(N-formyl-N-methyl)amino analogue, and the 8,9-Z isomer. The dc-ELISA reacted with these compounds at ratios of 113, 55, 38, and 9.1% of the IC(50) value of emamectin benzoate. Seven kinds of vegetables were spiked with emamectin benzoate at concentrations of 15-300 ng/g, and the recoveries were 91-117% in the dc-ELISA. The dc-ELISA results agreed reasonably well with results obtained by liquid chromatography-tandem mass spectrometry (LC-MS/MS) using spiked samples and actual (incurred) samples. The results indicate that the dc-ELISA was useful for the analysis of emamectin benzoate residues in agricultural products.

  1. Pesticide residues in leafy vegetables, stalk and stem vegetables from South Korea: a long-term study on safety and health risk assessment.

    PubMed

    Park, Duck Woong; Kim, Kwang Gon; Choi, Eun Ah; Kang, Gyeong Ri; Kim, Tae Sun; Yang, Yong Shik; Moon, Su Jin; Ha, Dong Ryong; Kim, Eun Sun; Cho, Bae Sik

    2016-01-01

    South Korea has a unique food culture. South Koreans enjoy wrapping meat and eating or making kimchi (traditionally fermented Korean food) and eating using raw leafy vegetables, stalk and stem vegetables. Therefore, there is a high chance of being exposed to pesticide residues of vegetables. The objective of this study was to investigate pesticide residues in leafy vegetables, stalk and stem vegetables from South Korea. A total of 8496 samples were mainly collected from Gwangju and Jeonnam area (the largest production region of leafy vegetables, stalk and stem vegetables) in South Korea from 2010 to 2014. A total of 230 pesticides were used for multi-residue analysis of pesticides. Among 8496 samples, 61 different pesticides (1029 times) were detected in 890 samples, of which 118 samples (1.4%) exceeded the Korea maximum residue limits (MRLs). Samples exceeding the MRLs were mostly found in leafy vegetables (brassica lee ssp. namai, leafy lettuce, spinach, perilla leaves, crown daisy, marsh mallow, aster scaber, pimpinella brachycarpa) and Chinese chive. Procymidone, dimethomorph and azoxystrobin were the most frequently found pesticides. A risk assessment of pesticides exceeding the MRLs was evaluated by calculating the estimated daily intake (EDI) and the acceptable daily intake (ADI). The ratio of EDI to ADI was 0.003-30.4%.

  2. Dissipation and Residues of Pyrethrins in Leaf Lettuce under Greenhouse and Open Field Conditions

    PubMed Central

    Pan, Lixiang; Feng, Xiaoxiao; Zhang, Hongyan

    2017-01-01

    Pyrethrins are nowadays widely used for prevention and control of insects in leaf lettuce. However, there is a concern about the pesticide residue in leaf lettuce. A reliable analytical method for determination of pyrethrins (pyrethrin—and П, cinerin І and П, and jasmolin І and П) in leaf lettuce was developed by using gas chromatography–mass spectrometry (GC–MS). Recoveries of pyrethrins in leaf lettuce at three spiking levels were 99.4–104.0% with relative standard deviations of 0.9–3.1% (n = 5). Evaluation of dissipation and final residues of pyrethrins in leaf lettuce were determined at six different locations, including the open field, as well as under greenhouse conditions. The initial concentration of pyrethrins in greenhouse (0.57 mg/kg) was higher than in open field (0.25 mg/kg) and the half-life for pyrethrins disappearance in field lettuce (0.7 days) was less than that greenhouse lettuce (1.1 days). Factors such as rainfall, solar radiation, wind speed, and crop growth rate are likely to have caused these results. The final residue in leaf lettuce was far below the maximum residue limits (MRLs) (1 mg/kg established by the European Union (EU), Australia, Korea, Japan). PMID:28754023

  3. 40 CFR 180.505 - Emamectin; tolerances for residues.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 25 2012-07-01 2012-07-01 false Emamectin; tolerances for residues... § 180.505 Emamectin; tolerances for residues. (a) General. (1) Tolerances are established for combined residues of emamectin (a mixture of a minimum of 90% 4′-epi-methylamino-4′-deoxyavermectin B1a and maximum...

  4. Properties of Arctic Aerosol Particles and Residuals of Warm Clouds: Cloud Activation Efficiency and the Aerosol Indirect Effect

    NASA Astrophysics Data System (ADS)

    Zelenyuk, A.; Imre, D. G.; Leaitch, R.; Ovchinnikov, M.; Liu, P.; Macdonald, A.; Strapp, W.; Ghan, S. J.; Earle, M. E.

    2012-12-01

    Single particle mass spectrometer, SPLAT II, was used to characterize the size, composition, number concentration, density, and shape of individual Arctic spring aerosol. Background particles, particles above and below the cloud, cloud droplet residuals, and interstitial particles were characterized with goal to identify the properties that separate cloud condensation nuclei (CCN) from background aerosol particles. The analysis offers a comparison between warm clouds formed on clean and polluted days, with clean days having maximum particle concentrations (Na) lower than ~250 cm-3, as compared with polluted days, in which maximum concentration was tenfold higher. On clean days, particles were composed of organics, organics mixed with sulfates, biomass burning (BB), sea salt (SS), and few soot and dust particles. On polluted days, BB, organics associated with BB, and their mixtures with sulfate dominated particle compositions. Based on the measured compositions and size distributions of cloud droplet residuals, background aerosols, and interstitial particles, we conclude that these three particle types had virtually the same compositions, which means that cloud activation probabilities were surprisingly nearly composition independent. Moreover, these conclusions hold in cases in which less than 20% or more than 90% of background particles got activated. We concluded that for the warm clouds interrogated in this study particle size played a more important factor on aerosol CCN activity. Comparative analysis of all studied clouds reveals that aerosol activation efficiency strongly depends on the aerosol concentrations, such that at Na <200 cm-3, nearly all particles activate, and at higher concentrations the activation efficiency is lower. For example, when Na was greater than 1500 cm-3, less than ~30% of particles activated. The data suggest that as the number of nucleated droplets increases, condensation on existing droplets effectively competes with particle activation, limiting maximum droplet concentrations Nd = 525 ± 50 cm-3, which is lower than the 750 cm-3 limit found by Leaitch et al. (1986) for mid-latitude continental cloud that had generally larger updraft speeds than the clouds interrogated in Arctic. These findings are important for the aerosol indirect effect, in which increase in aerosol particle number concentrations is expected to result in increase in Nd and decrease in droplet size, leading to increased cloud albedo and potentially lifetimes. Our conclusions point to limited susceptibility to changes in ambient aerosol concentrations, providing simple explanation for the finding of weaker than expected indirect effect. In summary, the data presented here show that Nd increases as the cloud base particle number concentration increases; however, they also show a limit on Nd that is in the range of 500-600 cm-3.

  5. Characteristics of the LacTek test as applied to tissue samples: assessment of performance using incurred field samples.

    PubMed

    Mitchell, J M; McNab, W B; Yee, A J; Griffiths, M W; McEwen, S A; Spilsbury, L; Boison, J O

    1998-08-01

    The Lactek test, marketed for antimicrobial residue detection in milk, was validated for the detection of antimicrobial residues in tissues. A previous study found that the LacTek test could confidently identify tissue samples spiked with antimicrobial residues. However, the test could not reliably distinguish violative from nonviolative spiked samples relative to Canadian maximum residue limits (MRLs). The objectives of this study were to assess and compare the performance of the LacTek tests for beta-lactams, tetracyclines, gentamicin, and sulfamethazine on samples containing naturally incurred residues by running the test in parallel with the standard microbial inhibition test (MIT) presently used for the routine testing of tissues at our facility and to assess the agreement with high pressure liquid chromatographic (HPLC) determinative methods. Parallel testing with the official MIT found that the Lactek tests could be confidently used for testing tissue samples containing incurred residues. Among 1,008 MIT-positive samples, the LacTek test found that 90% contained beta-lactams and/or tetracyclines. A further 7.3% of violative residues could not be identified to an antimicrobial class. In addition, 9% of samples testing negative on the MIT were found to contain an antimicrobial residue by the LacTek tests. Comparative testing with HPLC methods found that there was very good agreement between the two tests and that most violations were due to penicillin G and oxytetracycline. Although the LacTek test cannot be used to distinguish violative from nonviolative residue levels, it does offer several advantages over the present MIT. These include speed, ease of use, the ability to identify residues to a specific class, and an improved sensitivity at the MRL level for the most commonly found antimicrobials in tissue.

  6. Laboratory Evaluation of Residual Efficacy of Actellic 300 CS (Pirimiphos-Methyl) and K-Othrine WG 250 (Deltamethrin) on Different Indoor Surfaces.

    PubMed

    Ibrahim, Kolade T; Popoola, Kehinde O; Akure, Kenneth O

    2017-01-01

    The nature and type of local indoor resting wall surfaces to certain level influences the residual bio-efficacy of insecticides used in indoor residual spraying programs. Knockdown and mortality effects of an organophosphate Actellic 300 CS and pyrethroid K-Othrine WG 250 insecticides on the field-collected Culex quinquefasciatus were assessed bimonthly from July to November 2014, using World Health Organization (WHO) cones bioassay test. Knockdown and mortality rates were subjected to statistical analysis using χ 2 and Student t tests. Result of the bioassay test on C quinquefasciatus showed that plywood surfaces had the best residual knockdown activity of Actellic 300 CS with knockdown rate above the WHO-recommended threshold limit of ≥95% for 30 days after treatment. This was followed by mud surface with knockdown rates ≥95% threshold limit 15 days (97%) after treatment. The lowest knockdown rates of less than 95% were observed on cement surface throughout the assessment period. However, the knockdown rates of mosquitoes on deltamethrin WG 250-treated cement and plywood surfaces were 100% and ≥95%, respectively, at 30 days after treatment. But the knockdown activity was below the recommended threshold limit on mud surface during the 17 weeks trial. Knockdown activities varied significantly ( p  < .05), and it is a function of exposure periods, different surfaces, and insecticide formulations. The 24-hour mortality rates of Actellic 300 CS and K-Othrine WG 250 at 120 days after treatment were 83.6% and 86.7%, and 80% and 83.3%, on plywood and cement surfaces, respectively. A maximum residual period of 75 and 45 days were recorded for Actellic 300 CS and K-Othrine WG 250, respectively, on mud surface. Both Actellic 300 CS and K-Othrine 250 WG were highly effective against Culex mosquito. The extended residual activity of p -methyl CS compared with deltamethrin WG 250 makes it a suitable alternative insecticide against pyrethroid-resistant mosquitoes in Southwest Nigeria.

  7. Dissipation, residues and risk assessment of spirotetramat and its four metabolites in citrus and soil under field conditions by LC-MS/MS.

    PubMed

    Zhang, Qingtao; Chen, Yuling; Wang, Shouyi; Yu, Yurong; Lu, Ping; Hu, Deyu; Yang, Zaihui

    2018-04-01

    A modified Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for the simultaneous determination of spirotetramat and its four metabolite residues in citrus, peel, pulp and soil was developed and validated by liquid chromatography with tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile (1%, glacial acetic acid, v/v) and purified using primary secondary amine and octadecylsilane. The limit of detection was 0.01-0.13 mg/kg, whereas that of quantification was 0.02-0.40 mg/kg for spirotetramat and its metabolites. The average recoveries of spirotetramat, spirotetramat-enol, spirotetramat-mono-hydroxy, spirotetramat-enol-glucoside and spirotetramat-ketohydroxy in all matrices were 73.33-107.91%, 75.93-114.85%, 76.44-100.78%, 71.46-103.19% and 73.08-105.27%, respectively, with relative standard deviations < 12.32%. The dissipation dynamics of spirotetramat in citrus and soil followed first-order kinetics, with half-lives of 2.3-8.5 days in the three sampling locations. The terminal residues of spirotetramat in four matrices at the three locations were measured below the 1.0 mg/kg maximum residue limit set by China, and residues were found to be concentrated on the peel. The risk assessment of citrus was evaluated using risk quotients. The risk quotient values were found to be significantly <1, suggesting that the risk to human health was negligible when using the recommended doses of spirotetramat in citrus. These results could provide guidance for the safe and proper application of spirotetramat in citrus in China. Copyright © 2017 John Wiley & Sons, Ltd.

  8. Effective management tools for participants at Codex Committee on Residues of Veterinary Drugs meetings.

    PubMed

    Kay, Jack F

    2016-05-01

    The Codex Committee on Residues of Veterinary Drugs in Food (CCRVDF) fulfils a number of functions revolving around standard setting. The core activities of the CCRVDF include agreeing priorities for assessing veterinary drug residues, recommending maximum residue limits for veterinary drugs in foods of animal origin, considering methods of sampling and analyses, and developing codes of practice. Draft standards are developed and progress through an agreed series of steps common to all Codex Alimentarius Commission Committees. Meetings of the CCRVDF are held at approximately 18-month intervals. To ensure effective progress is made with meetings at this frequency, the CCRVDF makes use of a number of management tools. These include circular letters to interested parties, physical and electronic drafting groups between plenary sessions, meetings of interested parties immediately prior to sessions, as well as break out groups within sessions and detailed discussions within the CCRVDF plenary sessions. A range of these approaches is required to assist advances within the standards setting process and can be applied to other Codex areas and international standard setting more generally. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  9. Occurrence of agrochemical residues in beeswax samples collected in Italy during 2013-2015.

    PubMed

    Perugini, Monia; Tulini, Serena M R; Zezza, Daniela; Fenucci, Stefano; Conte, Annamaria; Amorena, Michele

    2018-06-01

    Considering the importance of honey bees for pollination activity and biodiversity preservation different studies have dealt with the impact of pesticides on honeybee health. Within the hive, beeswax is a matrix of particular interest because most of the chemicals used in agricultural and beekeeping activities can easily accumulate and persist in this matrix long after treatment has ceased, affecting honeybees survival. However, chemical analyses of pesticide residues in beeswax are not mandatory, so there are no residue limits, for beeswax. The present study was carried out with the aim of investigating the beeswax residue pattern in the Italian hives. 178 beeswax samples collected from 2013 to 2015 were analyzed for 247 pesticides. 73.6% of the analyzed samples reported the presence of one or more pesticides. On average every single sample showed a mean of three different pesticides each with a maximum of fourteen compounds, some of which were banned in Europe or not authorized in Italy. The higher frequencies were associated with three acaricides: coumaphos (60.7% of samples), tau-fluvalinate (50%) and chlorphenvinphos (35.4%), but the higher concentrations were associated to pyrethrins and piperonil butoxide. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Evaluation of Self-Propelled High-Energy Ultrasonic Atomizer on Azoxystrobin and Tebuconazole Application in Sunlit Greenhouse Tomatoes.

    PubMed

    Li, Yan-Jie; Li, Yi-Fan; Chen, Rong-Hua; Li, Xue-Sheng; Pan, Can-Ping; Song, Jian-Li

    2018-05-28

    In this study, a self-propelled high-energy ultrasonic atomizer was evaluated in terms of deposition on the canopy, the loss to the ground, and fungicide residues in cherry tomato and tomato. Artificial collectors fixed to the upper side and underside of the leaves at different depths and heights were used to collect the depositions. A reliable analytical method for determination of azoxystrobin and tebuconazole in artificial collectors and residue samples was developed by using liquid chromatography triple-quadrupole mass spectrometry. The results showed that the atomizer distributed the droplets evenly throughout the greenhouse with good uniformity (CVs below 39%). The ratio of depositions on the internal and external sides was 66⁻83%, and the ratio of depositions on the underside and upper side was 39⁻50%. There were no significant differences in depositions between two different height crops. The residues of azoxystrobin and tebuconazole in tomato and cherry tomato fruits were far below the maximum residue limits at harvest time. In general, self-propelled high-energy ultrasonic atomizer used in a greenhouse could increase the depositions, especially on the underside and internal side of the canopies, and lead to a reduction of operator exposure risk.

  11. Toxicity and bioconcentration evaluation of RDX and HMX using sheepshead minnows in water exposures.

    PubMed

    Lotufo, Guilherme R; Gibson, Alfreda B; Yoo, J Leslie

    2010-10-01

    Lethal effects of the explosives RDX and HMX were assessed using ten-day water exposures to juvenile sheepshead minnows (Cyprinodon variegatus). For RDX, maximum mortality occurred during the first two days of exposure with a 10-d median lethal concentration (LC50) of 9.9 mg L(-1). The RDX 10-d median lethal residue (LR50) was 9.6 mg kg(-1) (34.9 μmol kg(-1)) wet weight (ww), the first RDX critical body residue reported for fish. Previous investigations reported that RDX body residues in marine amphipods up to 96 μmol kg(-1) ww and in marine mussels up to 86 μmol kg(-1) ww failed to result in significant mortality. The highest HMX concentration tested, corresponding to its apparent solubility limit in seawater (2.0 mg L(-1)), and the associated mean body residue (3 mg kg(-1) or 14 μmol kg(-1) ww) resulted in no significant mortality for exposed minnows. The mean 10-d bioconcentration factors for RDX (0.6-0.9 L kg(-1)) and HMX (0.3-1.6 L kg(-1)) were typically lower than 1, reflecting the low bioaccumulative potential for these compounds. Published by Elsevier Inc.

  12. Occurrence and human dietary assessment of fluoroquinolones antibiotics in cultured fish around tai lake, China.

    PubMed

    Song, Chao; Zhang, Cong; Kamira, Barry; Qiu, Liping; Fan, Limin; Wu, Wei; Meng, Shunlong; Hu, Gengdong; Chen, Jiazhang

    2017-11-01

    Fluoroquinolone antibiotics are widely used in the production of aquatic products and considered to be a significant contributing factor to the burden of both natural and aquaculture environments. However, the main types of fluoroquinolones present in aquaculture systems have not been determined. The objectives of the present study were to explore the occurrence of residual fluoroquinolone antibiotics in fish muscle tissues sampled from across the entire aquaculture season in the Tai Lake basin in China and to assess the dietary risks associated with the upcoming vendible fish in the last month of the aquaculture season. Fluoroquinolones were detected in 95.69% of all fish samples, and the concentrations ranged from the limit of quantification (LOQ) to 47 108.00 μg · kg -1 . Enrofloxacin contributed the most among the 9 fluoroquinolone antibiotics tested. Of the 4 fish species studied, enrofloxacin was present in bream at significant (p < 0.05) concentrations in August, with an average value of 321.45 μg · kg -1 , while enrofloxacin concentrations peaked in crab and shrimp in September, with average values of 6949.60 and 460.82 μg · kg -1 , respectively. However, different patterns were observed in perch, suggesting that other categories of antibiotics may be used in the production of this fish. Dietary risk assessment showed that the residual levels and estimated daily intake in bream, perch, and shrimp were far below the maximum residual level and acceptable daily intake. However, the average residual level in crab exceeded the maximum residual level, and the estimated daily intake value accounted for 78.49% of the acceptable daily intake, indicating potential consumption risk. In summary, the present study aims to guide the production and consumption of aquatic products. Environ Toxicol Chem 2017;36:2899-2905. © 2017 SETAC. © 2017 SETAC.

  13. Research on disposal of copper(II)-containing wastewater by secondary strontium residue

    NASA Astrophysics Data System (ADS)

    Qing, Duowen; Xu, Longjun; Cui, Caixi

    2018-01-01

    Secondary strontium residue (SSR) was used as absorbent to remove Cu2+ in solution and the effects of experimental conditions on absorption of Cu2+ were investigated. The results showed that the absorption process reached balance in around 40 min. The absorption capacity achieved the maximum when PH value reached 6, and the maximum adsorption of Cu2+-containing wastewater by secondary strontium residue was 5.46 mg/g. Removal ratio of Cu2+ was in relation to initial concentration of Cu2+ in solution. Adsorptive process tallied with Langmuir Isothermal adsorption model.

  14. Residual toxicity of Cypermethrin in the larvae of coconut pest Oryctes rhinoceros (Coleoptera: Scarabaeidae).

    PubMed

    Venkatarajappa, P

    2001-01-01

    The toxic effect of Cypermethrin 10 EC (0.125, 0.25 and 0.5%) was estimated in the bodywall and digestive system of the larvae of Oryctes rhinoceros by HPLC after exposing them to different concentrations (0.125, 0.25 and 0.5%). Among the various concentrations used maximum residues were detected in bodywall (0.25%), whereas at higher concentration (0.5%) the residue detected was minimum. The treatment of Cypermethrin was found to be highly toxic upto 12 h of treatment, after which it declined reaching the minimum by 24 h. The residue of Cypermethrin could not be detected in digestive system. The experiments indicate the pesticide get concentrated in the bodywall to a maximum extent.

  15. 21 CFR 178.3530 - Isoparaffinic petroleum hydrocarbons, synthetic.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... millimicrons—1.5 maximum. 320-329 millimicrons—0.08 maximum. 330-350 millimicrons—0.05 maximum. Nonvolatile residue 0.002 gram per 100 milliliters maximum. Synthetic isoparaffinic petroleum hydrocarbons containing... from the American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia...

  16. The effect of motorcycle helmet fit on estimating head impact kinematics from residual liner crush.

    PubMed

    Bonin, Stephanie J; Gardiner, John C; Onar-Thomas, Arzu; Asfour, Shihab S; Siegmund, Gunter P

    2017-09-01

    Proper helmet fit is important for optimizing head protection during an impact, yet many motorcyclists wear helmets that do not properly fit their heads. The goals of this study are i) to quantify how a mismatch in headform size and motorcycle helmet size affects headform peak acceleration and head injury criteria (HIC), and ii) to determine if peak acceleration, HIC, and impact speed can be estimated from the foam liner's maximum residual crush depth or residual crush volume. Shorty-style helmets (4 sizes of a single model) were tested on instrumented headforms (4 sizes) during linear impacts between 2.0 and 10.5m/s to the forehead region. Helmets were CT scanned to quantify residual crush depth and volume. Separate linear regression models were used to quantify how the response variables (peak acceleration (g), HIC, and impact speed (m/s)) were related to the predictor variables (maximum crush depth (mm), crush volume (cm 3 ), and the difference in circumference between the helmet and headform (cm)). Overall, we found that increasingly oversized helmets reduced peak headform acceleration and HIC for a given impact speed for maximum residual crush depths less than 7.9mm and residual crush volume less than 40cm 3 . Below these levels of residual crush, we found that peak headform acceleration, HIC, and impact speed can be estimated from a helmet's residual crush. Above these crush thresholds, large variations in headform kinematics are present, possibly related to densification of the foam liner during the impact. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Validation of QuEChERS method for the determination of some pesticide residues in two apple varieties.

    PubMed

    Tiryaki, Osman

    2016-10-02

    This study was undertaken to validate the "quick, easy, cheap, effective, rugged and safe" (QuEChERS) method using Golden Delicious and Starking Delicious apple matrices spiked at 0.1 maximum residue limit (MRL), 1.0 MRL and 10 MRL levels of the four pesticides (chlorpyrifos, dimethoate, indoxacarb and imidacloprid). For the extraction and cleanup, original QuEChERS method was followed, then the samples were subjected to liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) for chromatographic analyses. According to t test, matrix effect was not significant for chlorpyrifos in both sample matrices, but it was significant for dimethoate, indoxacarb and imidacloprid in both sample matrices. Thus, matrix-matched calibration (MC) was used to compensate matrix effect and quantifications were carried out by using MC. The overall recovery of the method was 90.15% with a relative standard deviation of 13.27% (n = 330). Estimated method detection limit of analytes blew the MRLs. Some other parameters of the method validation, such as recovery, precision, accuracy and linearity were found to be within the required ranges.

  18. Rapid method for quantification of nine sulfonamides in bovine milk using HPLC/MS/MS and without using SPE.

    PubMed

    Nebot, Carolina; Regal, Patricia; Miranda, Jose Manuel; Fente, Cristina; Cepeda, Alberto

    2013-12-01

    Sulfonamides are antimicrobial agents widely employed in animal production and their residues in food could be an important risk to human health. In the dairy industry, large quantities of milk are monitored daily for the presence of sulfonamides. A simple and low-cost extraction protocol followed by a liquid chromatographic-tandem mass spectrometry method was developed for the simultaneous detection of nine sulfonamides in whole milk. The method was validated at the maximum residue limits established by European legislation. The limits of quantification obtained for most sulfonamides were between 12.5 and 25 μg kg(-1), detection capabilities ranged from 116 to 145 μg kg(-1), and recoveries, at 100 μg kg(-1), were greater than 89±12.5%. The method was employed to analyse 100 raw whole bovine milk samples collected from dairy farms in the northwest region of Spain. All of the samples were found to be compliant, but two were positive; one for sulfadiazine and the other for sulfamethoxipyridazine. Copyright © 2013 Elsevier Ltd. All rights reserved.

  19. Antibiotic use in heavy pigs: Comparison between urine and muscle samples from food chain animals analysed by HPLC-MS/MS.

    PubMed

    Chiesa, Luca Maria; Nobile, Maria; Panseri, Sara; Arioli, Francesco

    2017-11-15

    The antibiotic overuse in zoothechnics, due to prophylactic and therapeutic treatments, or to their growth-promoting activity, is a major cause for the onset of widespread antibiotic resistance. Of particular relevance to this study, is the antibiotic abuse in pig breeding. Despite the comprehensive literature on residue controls in pig muscle, data on pig urine, a non-invasive, on-farm collectable matrix, are lacking. Therefore, we validated an HPLC-MS/MS method to detect 29 antimicrobials from eight classes and applied it to 43 anonymous pig urine and muscle paired samples and fulfilled the parameters in agreement with the Commission Decision 2002/657/UE. The analytical limits were moreover much lower than the maximum residue limits (MRLs) required by the Commission Regulation 37/2010/UE. In the samples, antibiotics were usually detected at higher frequencies and concentrations in urine than muscle. Urine proved a useful tool to detect antibiotic administration and their excessive use in pig farming is depicted. Copyright © 2017. Published by Elsevier Ltd.

  20. Analytical methods for multiresidue determination of sulfonamides and trimethoprim in meat and ground water samples by CE-MS and CE-MS/MS.

    PubMed

    Soto-Chinchilla, Jorge J; García-Campaña, Ana M; Gámiz-Gracia, Laura

    2007-11-01

    This paper presents two methods based on CZE-MS detection and CZE-MS/MS detection developed for the multiresidue determination of ten sulfonamides (sulfapyridine, sulfadoxin, sulfamethazine, sulfadimethoxine, sulfameter, sulfamerazine, sulfachlorpyridazine, sulfadiazine, sulfamethoxazole, and sulfamethizole) and a potentiator, trimethoprim (TMP), whose contents are regulated by the EU Council Regulation no. 2377/90 in animal edible tissues. Experimental designs were employed to optimize the electrospray conditions. MS/MS experiments using an IT as analyzer operating in multiple reaction monitoring (MRM) mode were carried out to achieve the minimum number of points according to the 2002/657/EC European Decision for unambiguous identification. The proposed procedures have been compared in terms of the performance characteristics and trueness. The limits of detection and quantification were in all cases lower than the maximum residue limits legislated for these compounds and the recoveries were satisfactory, being possible the application for their monitoring in foodstuff of animal origin and in environmental samples, allowing the determination of sulfonamides and TMP residues in meat and in superficial water in the low microg/L range.

  1. The response of meat ducks from 15 to 35 d of age to gossypol from cottonseed meal

    PubMed Central

    Zeng, Q. F.; Bai, P.; Wang, J. P.; Ding, X. M.; Luo, Y. H.; Bai, S. P.; Xuan, Y.; Su, Z. W.; Lin, S. Q.; Zhao, L. J.; Zhang, K. Y.

    2015-01-01

    The objective of this study was to investigate the responses of meat ducks of 15 to 35 d of age to free gossypol (FG) from cottonseed meal (CSM) and to establish the maximum limits of dietary FG concentration based on growth performance, blood parameters, and tissue residues of gossypol. Nine hundred 15-d-old ducks were randomly allocated to 5 treatments with 10 cages/treatment and 18 ducks/cage on the basis of BW. Five isonitrogenous and isocaloric experimental diets were formulated on a digestible amino acid basis to produce diets in which 0% (without FG), 25% (36 mg FG/kg), 50% (75 mg FG/kg), 75% (111 mg FG/kg), and 100% (153 mg FG/kg) of protein from soybean meal were replaced by that from CSM. Increasing dietary FG content, BW, and ADG decreased (linearly, P < 0.05, except for ADG of days 29 to 35), and F/G linearly increased (P < 0.05). At 35 d, blood hemoglobin, mean corpuscular hemoglobin, and mean corpuscular hemoglobin concentration linearly decreased (P < 0.05), while serum total protein, albumin, and globulin content linearly decreased (P < 0.05), and the residue of gossypol in liver, kidney, heart, breast, and leg muscle linearly increased (P < 0.001) with increases in dietary FG concentration. Ducks fed 36 mg FG/kg (5.83% CSM of diet) diet had a normal histological structure of liver, and muscle (breast and leg) had no residue of gossypol. The maximum limit of dietary FG concentration was estimated to range from a low of 36 mg/kg to maximize serum globulin concentration to a high of 124 mg/kg to minimize feed intake for 22 to 28d on the basis of a quadratic broken-line model. PMID:25834247

  2. The response of meat ducks from 15 to 35 d of age to gossypol from cottonseed meal.

    PubMed

    Zeng, Q F; Bai, P; Wang, J P; Ding, X M; Luo, Y H; Bai, S P; Xuan, Y; Su, Z W; Lin, S Q; Zhao, L J; Zhang, K Y

    2015-06-01

    The objective of this study was to investigate the responses of meat ducks of 15 to 35 d of age to free gossypol (FG) from cottonseed meal (CSM) and to establish the maximum limits of dietary FG concentration based on growth performance, blood parameters, and tissue residues of gossypol. Nine hundred 15-d-old ducks were randomly allocated to 5 treatments with 10 cages/treatment and 18 ducks/cage on the basis of BW. Five isonitrogenous and isocaloric experimental diets were formulated on a digestible amino acid basis to produce diets in which 0% (without FG), 25% (36 mg FG/kg), 50% (75 mg FG/kg), 75% (111 mg FG/kg), and 100% (153 mg FG/kg) of protein from soybean meal were replaced by that from CSM. Increasing dietary FG content, BW, and ADG decreased (linearly, P<0.05, except for ADG of days 29 to 35), and F/G linearly increased (P<0.05). At 35 d, blood hemoglobin, mean corpuscular hemoglobin, and mean corpuscular hemoglobin concentration linearly decreased (P<0.05), while serum total protein, albumin, and globulin content linearly decreased (P<0.05), and the residue of gossypol in liver, kidney, heart, breast, and leg muscle linearly increased (P<0.001) with increases in dietary FG concentration. Ducks fed 36 mg FG/kg (5.83% CSM of diet) diet had a normal histological structure of liver, and muscle (breast and leg) had no residue of gossypol. The maximum limit of dietary FG concentration was estimated to range from a low of 36 mg/kg to maximize serum globulin concentration to a high of 124 mg/kg to minimize feed intake for 22 to 28 d on the basis of a quadratic broken-line model. © The Author 2015. Published by Oxford University Press on behalf of Poultry Science Association.

  3. 21 CFR 178.3530 - Isoparaffinic petroleum hydrocarbons, synthetic.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... absorbance: 260-319 millimicrons—1.5 maximum. 320-329 millimicrons—0.08 maximum. 330-350 millimicrons—0.05 maximum. Nonvolatile residue 0.002 gram per 100 milliliters maximum. Synthetic isoparaffinic petroleum.... Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West...

  4. 21 CFR 178.3530 - Isoparaffinic petroleum hydrocarbons, synthetic.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... absorbance: 260-319 millimicrons—1.5 maximum. 320-329 millimicrons—0.08 maximum. 330-350 millimicrons—0.05 maximum. Nonvolatile residue 0.002 gram per 100 milliliters maximum. Synthetic isoparaffinic petroleum.... Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West...

  5. 21 CFR 172.882 - Synthetic isoparaffinic petroleum hydrocarbons.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... absorbance: 260-319 millimicrons—1.5 maximum. 320-329 millimicrons—0.08 maximum. 330-350 millimicrons—0.05 maximum. Nonvolatile residual: 0.002 gram per 100 milliliters maximum. Synthetic isoparaffinic petroleum... reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West...

  6. 21 CFR 172.882 - Synthetic isoparaffinic petroleum hydrocarbons.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... absorbance: 260-319 millimicrons—1.5 maximum. 320-329 millimicrons—0.08 maximum. 330-350 millimicrons—0.05 maximum. Nonvolatile residual: 0.002 gram per 100 milliliters maximum. Synthetic isoparaffinic petroleum... reference. Copies may be obtained from the American Society for Testing Materials, 100 Barr Harbor Dr., West...

  7. Impacts of alum residues from Morton Jaffray Water Works on water quality and fish, Harare, Zimbabwe

    NASA Astrophysics Data System (ADS)

    Muisa, Norah; Hoko, Zvikomborero; Chifamba, Portia

    Metal pollution of freshwater due to human activities is a major problem confronting most urban centres in developing countries. This study determined the extent to which aluminium in the residues from Morton Jaffray Water Works in Harare were affecting the water quality of Manyame River and Lake Manyame. The study also measured aluminium bioaccumulation in Nile Tilapia ( Oreochromis niloticus) which is of importance to the commercial fisheries industry in Zimbabwe. Depth integrated water, and sediment grab samples and adult fish were collected per site in January and March, 2010. A total of six sites were selected on the Manyame River and in Lake Manyame. The levels of Total Aluminium (Al) were determined in sediments, water and fish tissues (liver, kidney, gill and muscle). Total solids, total dissolved solids, conductivity, pH, dissolved oxygen and temperature were also determined in water and residues. The texture of the sediments was also assessed. Aluminium concentration in water ranged from 2.19 mg/L to 68.93 mg/L during both sampling campaigns surpassing permissible maximum concentration limits of 0.087 to 0.75 mg/L suggested by the Environmental Protection Agency and African Union. The site upstream of the discharge point of the residues always had the lowest levels though it was higher than acceptable levels indicated above, thus suggesting the existence of other sources of aluminium in the catchment besides Morton Jaffray Water Works. However, there was a 10-fold and 100-fold increase in levels of aluminium in water and sediments, respectively, at the site 100 m downstream of the discharge point on the Manyame River. Mean aluminium concentrations in water and sediments at this site averaged 68.93 ± 61.74 mg/L and 38.18 ± 21.54 mg/L in water and 103.79 ± 55.96 mg/L and 131.84 ± 16.48 mg/L in sediments in sampling campaigns 1 and 2, respectively. These levels were significantly higher than levels obtained from all the other sites during both sampling campaigns (ANOVA: p < 0.05). This also indicated that the contribution of aluminium pollution from the water works residues was higher than all the other sources in the catchment. Aluminium levels were generally in the order of; sediments > fish > water. Bioaccumulation occurred in the fish and the order of bioconcentration was; kidney > liver > gill > muscle. The amounts of aluminium in the fish tissues investigated were significantly higher (maximum = 2.92 mg/g) than was reported in other studies reviewed (maximum = 0.18 mg/g). Thus, the water treatment plant residues are greatly increasing the concentrations of aluminium in the water system downstream of the plant thus creating a great risk of aluminium toxicity for fish. Treatment of the residues before discharge, substitution of alum with other coagulants, and re-use of the residues in buffer strips, agricultural lands and in sewage works should be considered.

  8. Utilization of lignite power generation residues for the production of lightweight aggregates.

    PubMed

    Anagnostopoulos, Iason M; Stivanakis, Victor E

    2009-04-15

    A novel process is proposed for the utilization of lignite combustion solid residues in the production of inflammable lightweight aggregates (LWA). The process consists of two stages, pelletization and sintering, and carbon contained in BA was used as the process fuel. The main residues bottom ash (BA) and fly ash (FA) from Megalopolis power plant were characterized, mixed in different proportions and treated through pelletization and sintering process. Sintering benefits from combustion of BA carbon content and the product is a hardened porous cake. The energy required for achievement of high temperatures, in the range of 1250 degrees C, was offered by carbon combustion and CO(2) evolution is responsible for porous structure formation. Selected physical properties of sintered material relevant to use as lightweight aggregates were determined, including bulk density, porosity and water absorption. Bulk density varies from 0.83 to 0.91 g/cm(3), porosity varies from 60% to 64% and water absorption varies from 66% to 80%. LWA formed is used for the production of lightweight aggregate concrete (LWAC). Thermal conductivity coefficient varies from 0.25 to 0.37 W/mK (lower than maximum limit 0.43 W/mK) and compressive strength varies from 19 to 23 MPa (higher than minimum limit 17 MPa). The results indicate that sintering of lignite combustion residues is an efficient method of utilization of carbon containing BA and production of LWA for structural and insulating purposes. Carbon content of BA is a key factor in LWA production. Finally, this research work comprises the first proposed application for utilization of BA in Greece.

  9. A broad-scale comparison of aerobic activity levels in vertebrates: endotherms versus ectotherms

    PubMed Central

    Gomez, Juan Pablo; Mavrodiev, Evgeny V.

    2017-01-01

    Differences in the limits and range of aerobic activity levels between endotherms and ectotherms remain poorly understood, though such differences help explain basic differences in species' lifestyles (e.g. movement patterns, feeding modes, and interaction rates). We compare the limits and range of aerobic activity in endotherms (birds and mammals) and ectotherms (fishes, reptiles, and amphibians) by evaluating the body mass-dependence of VO2 max, aerobic scope, and heart mass in a phylogenetic context based on a newly constructed vertebrate supertree. Contrary to previous work, results show no significant differences in the body mass scaling of minimum and maximum oxygen consumption rates with body mass within endotherms or ectotherms. For a given body mass, resting rates and maximum rates were 24-fold and 30-fold lower, respectively, in ectotherms than endotherms. Factorial aerobic scope ranged from five to eight in both groups, with scope in endotherms showing a modest body mass-dependence. Finally, maximum consumption rates and aerobic scope were positively correlated with residual heart mass. Together, these results quantify similarities and differences in the potential for aerobic activity among ectotherms and endotherms from diverse environments. They provide insights into the models and mechanisms that may underlie the body mass-dependence of oxygen consumption. PMID:28202808

  10. Blind Bayesian restoration of adaptive optics telescope images using generalized Gaussian Markov random field models

    NASA Astrophysics Data System (ADS)

    Jeffs, Brian D.; Christou, Julian C.

    1998-09-01

    This paper addresses post processing for resolution enhancement of sequences of short exposure adaptive optics (AO) images of space objects. The unknown residual blur is removed using Bayesian maximum a posteriori blind image restoration techniques. In the problem formulation, both the true image and the unknown blur psf's are represented by the flexible generalized Gaussian Markov random field (GGMRF) model. The GGMRF probability density function provides a natural mechanism for expressing available prior information about the image and blur. Incorporating such prior knowledge in the deconvolution optimization is crucial for the success of blind restoration algorithms. For example, space objects often contain sharp edge boundaries and geometric structures, while the residual blur psf in the corresponding partially corrected AO image is spectrally band limited, and exhibits while the residual blur psf in the corresponding partially corrected AO image is spectrally band limited, and exhibits smoothed, random , texture-like features on a peaked central core. By properly choosing parameters, GGMRF models can accurately represent both the blur psf and the object, and serve to regularize the deconvolution problem. These two GGMRF models also serve as discriminator functions to separate blur and object in the solution. Algorithm performance is demonstrated with examples from synthetic AO images. Results indicate significant resolution enhancement when applied to partially corrected AO images. An efficient computational algorithm is described.

  11. Residual dynamic and risk assessment of dimethomorph in Swiss chard grown at two different sites.

    PubMed

    Kabir, Md Humayun; Abd El-Aty, A M; Rahman, Md Musfiqur; Chung, Hyung Suk; Lee, Han Sol; Kim, Mi-Ra; Chang, Byung-Joon; Wang, Jing; Shin, Ho-Chul; Shim, Jae-Han

    2018-02-01

    Residue analysis of dimethomorph in Swiss chard cultivated at two different locations under greenhouse conditions was conducted using high-performance liquid chromatography-ultraviolet detection and confirmed by tandem mass spectrometry. The randomly collected samples (over 14 days) were extracted with acetonitrile and purified using a Florisil solid-phase extraction cartridge. Linearity over a concentration range of 0.05-50.0 mg/L had an excellent coefficient of determination of 0.9996. Recovery rate ranged from 82.98 to 95.43% with relative standard deviations ≤5.12% and limits of detection and quantification of 0.003 and 0.01 mg/kg, respectively. The initial deposits [day 0 (2 h post-application)] were considerably lower (7.57 and 8.55 mg/kg for sites 1 and 2, respectively) than the maximum residue limit (30 mg/kg) set by the Korean Ministry of Food and Drug Safety. The dissipation half-life was approximately the same, being 5.0 and 5.1 days for sites 1 and 2, respectively. Risk assessment estimated as acceptable daily intake revealed a value of 0.084 or 0.094% (day 0) and 0.014% (10 days post-application), for sites 1 and 2, respectively. The values indicated that dimethomorph can be safely used on Swiss chard, with no hazardous effects expected for Korean consumers. Copyright © 2017 John Wiley & Sons, Ltd.

  12. Multilocation field trials for risk assessment of a combination fungicide Fluopicolide + Propamocarb in tomato.

    PubMed

    Sharma, K K; Shukla, V R; Patel, A R; Vaghela, K M; Patel, H K; Shah, Paresh G; Banerjee, Hemanta; Banerjee, Tirthankar; Hudait, Ram K; Sharma, Debi; Sahoo, S K; Singh, Balwinder; Tripathy, Vandana

    2016-11-01

    Dissipation kinetics of two systemic fungicides, namely fluopicolide and propamocarb used as a combination formulation (Infinito 68.75 SC), were studied on tomato at four different locations by the All India Network Project on Pesticide Residues to recommend their pre-harvest interval (PHI) and to propose the maximum residue limits (MRL) for the two fungicides based on chronic hazard exposure assessment. The combination fungicide was sprayed thrice at the recommended dosage of 93.75 g a.i./ha fluopicolide and 937.50 g a.i./ha propamocarb as well as at double the recommended dosage of 187.50 g a.i./ha fluopicolide and 1875.0 g a.i./ha propamocarb on tomato crops and the residues were monitored periodically by GC-MS. The fungicides dissipated to below the limit of quantification (LOQ) within 10 to 15 days, with a half-life of 2-4 days for fluopicolide and 1-2 days for propamocarb. Taking into consideration the MRLs of codex and calculations made using the method of MRL fixation of the Food Safety and Standard Authority of India (FSSAI) as well as the Organization for Economic Co-operation and Development (OECD) calculator, MRL of 5 mg/kg is proposed for fluopicolide and 15 mg/kg for propamocarb, following critical exposure of the commodity considering PHI of 1 day.

  13. Pesticide residues variability and acute dietary risk assessment: a consumer perspective.

    PubMed

    Lefferts, L Y

    2000-07-01

    In relation to residue variability and acute dietary intake, this paper considers whether or not consumers are adequately protected, and makes recommendations for governments and international bodies. Existing risk assessment science is inadequate to lay to rest some concerns raised by the scientific community, and it is plausible that acute exposures to pesticides from the most contaminated food may be causing adverse effects in some consumers. Consumers International recommends that: (1) analysis and regulation of pesticides with a common mechanism of action (e.g. organophosphate insecticides) be conducted in an integrated, aggregated manner, not on a single pesticide basis; (2) exposure to pesticides in foods consumed in large amounts by children be reduced by revising good agricultural practices; (3) clear risk assessment policies for acute risk assessments be established at the national and international level; and (4) an additional safety factor be applied in order to protect children when establishing maximum residue limits (MRLs) for pesticides in the absence of reliable data on the effects of pesticides on children (e.g. no pesticide-specific tests on immature animals for effects on the developing brain, endocrine, or immune systems).

  14. Recent Modifications and Validation of QuEChERS-dSPE Coupled to LC-MS and GC-MS Instruments for Determination of Pesticide/Agrochemical Residues in Fruits and Vegetables: Review.

    PubMed

    Lawal, Abubakar; Wong, Richard Chee Seng; Tan, Guan Huat; Abdulra'uf, Lukman Bola; Alsharif, Ali Mohamed Ali

    2018-04-21

    Fruits and vegetables constitute a major type of food consumed daily apart from whole grains. Unfortunately, the residual deposits of pesticides in these products are becoming a major health concern for human consumption. Consequently, the outcome of the long-term accumulation of pesticide residues has posed many health issues to both humans and animals in the environment. However, the residues have previously been determined using conventionally known techniques, which include liquid-liquid extraction, solid-phase extraction (SPE) and the recently used liquid-phase microextraction techniques. Despite the positive technological effects of these methods, their limitations include; time-consuming, operational difficulty, use of toxic organic solvents, low selective property and expensive extraction setups, with shorter lifespan of instrumental performances. Thus, the potential and maximum use of these methods for pesticides residue determination has resulted in the urgent need for better techniques that will overcome the highlighted drawbacks. Alternatively, attention has been drawn recently towards the use of quick, easy, cheap, effective, rugged and safe technique (QuEChERS) coupled with dispersive solid-phase extraction (dSPE) to overcome the setback challenges experienced by the previous technologies. Conclusively, the reviewed QuEChERS-dSPE techniques and the recent cleanup modifications justifiably prove to be reliable for routine determination and monitoring the concentration levels of pesticide residues using advanced instruments such as high-performance liquid chromatography, liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry.

  15. A simple, fast and cheap non-SPE screening method for antibacterial residue analysis in milk and liver using liquid chromatography-tandem mass spectrometry.

    PubMed

    Martins, Magda Targa; Melo, Jéssica; Barreto, Fabiano; Hoff, Rodrigo Barcellos; Jank, Louise; Bittencourt, Michele Soares; Arsand, Juliana Bazzan; Schapoval, Elfrides Eva Scherman

    2014-11-01

    In routine laboratory work, screening methods for multiclass analysis can process a large number of samples in a short time. The main challenge is to develop a methodology to detect as many different classes of residues as possible, combined with speed and low cost. An efficient technique for the analysis of multiclass antibacterial residues (fluoroquinolones, tetracyclines, sulfonamides and trimethoprim) was developed based on simple, environment-friendly extraction for bovine milk, cattle and poultry liver. Acidified ethanol was used as an extracting solvent for milk samples. Liver samples were treated using EDTA-washed sand for cell disruption, methanol:water and acidified acetonitrile as extracting solvent. A total of 24 antibacterial residues were detected and confirmed using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS), at levels between 10, 25 and 50% of the maximum residue limit (MRL). For liver samples a metabolite (sulfaquinoxaline-OH) was also monitored. A validation procedure was conducted for screening purposes in accordance with European Union requirements (2002/657/EC). The detection capability (CCβ) false compliant rate was less than 5% at the lowest level for each residue. Specificity and ruggedness were also discussed. Incurred and routine samples were analyzed and the method was successfully applied. The results proved that this method can be an important tool in routine analysis, since it is very fast and reliable. Copyright © 2014. Published by Elsevier B.V.

  16. Monitoring of selected pesticides residue levels in water samples of paddy fields and removal of cypermethrin and chlorpyrifos residues from water using rice bran.

    PubMed

    Bhattacharjee, Shubhra; Fakhruddin, A N M; Chowdhury, M A Z; Rahman, M A; Alam, M K

    2012-08-01

    Consumption of pesticides associated foods increased in recent decades in Bangladesh. Most of the pesticides come from paddy, as rice is the main food items here and about 70 % pesticides are used only on paddy fields. Water samples of paddy fields and Kaliganga River of Manikganj district were analyzed to provide base line data on cypermethrin, chlorpyrifos and diazinon residue by using high performance liquid chromatography. Levels of Cypermethrin, chlorpyrifos and diazinon detected in the paddy field water samples were (0.605 ± 0.011 μg/L), (0.06 ± 0.001 μg/L) and (0.039 ± 0.002 μg/L), respectively. 0.11 ± 0.003 μg/L of cypermethrin and 0.012 ± 0.0006 μg/L of chlorpyrifos were also identified in the water samples of Kaligonga River. Diazinon residue was not detected in the river water samples. The detected concentrations of pesticide residues in the river water were below the accepted maximum residue limit (MRL) value of drinking water (0.1 μg/l) adopted by the FAO/WHO Codex Alimentarius Commission. Cypermethrin and chlorpyrifos were chosen for decontamination through rice bran, as it was found in river water. Two gm rice bran could easily decontaminated 95.6 % and 96.4 % of cypermethrin and chlorpyrifos. The result of this study showed that pesticide residue was detected in water samples were below the MRLs value, which can easily be decontaminated through absorption of rice bran.

  17. Dynamic contrast-enhanced MRA at 1.5 T for detection of arteriovenous shunting before and after Onyx embolization of cerebral arteriovenous malformations.

    PubMed

    Nogueira, Raul G; Bayrlee, Ahmad; Hirsch, Joshua A; Yoo, Albert J; Copen, William A

    2013-10-01

    Conventional non-invasive angiographic techniques for evaluating cerebral Arteriovenous Malformations (cAVMs) after embolization treatment are limited by their inability to acquire time-resolved images. We describe the use of dynamic contrast-enhanced magnetic resonance angiography (MRA) in the evaluation of residual arteriovenous shunting in cAVMs following Onyx embolization. Six subjects who underwent multimodal MR imaging including dynamic MRA after different stages of endovascular treatment with Onyx were included. Each MRA was assessed for the presence of residual arteriovenous shunting. The results were compared with digital subtraction angiography (DSA). Mean age was 41 years (range, 25-63) and the mean maximum AVM diameter was 5.3 cm (range, 4.7-6.0). Fourteen dynamic MRA were performed using a 1.5 T scanner. Arteriovenous shunting was detected in thirteen of fourteen patients by both dynamic MRA and DSA, with complete agreement between the two techniques. The only MRA without detectable residual arteriovenous shunting was for a subject who had complete treatment with no residual cAVM as confirmed by the DSA images. Dynamic contrast-enhanced MRA is a promising non-invasive modality in identifying residual arteriovenous shunting after different stages of AVM embolization, achieving 100% agreement in this small study. Embolization with Onyx caused no significant image artifact. Copyright © 2013 by the American Society of Neuroimaging.

  18. Measuring dry plant residues in grasslands: A case study using AVIRIS

    NASA Technical Reports Server (NTRS)

    Fitzgerald, Michael; Ustin, Susan L.

    1992-01-01

    Grasslands, savannah, and hardwood rangelands are critical ecosystems and sensitive to disturbance. Approximately 20 percent of the Earth's surface are grasslands and represent 3 million ha. in California alone. Developing a methodology for estimating disturbance and the effects of cumulative impacts on grasslands and rangelands is needed to effectively monitor these ecosystems. Estimating the dry biomass residue remaining on rangelands at the end of the growing season provides a basis for evaluating the effectiveness of land management practices. The residual biomass is indicative of the grazing pressure and provides a measure of the system capacity for nutrient cycling since it represents the maximum organic matter available for decomposition, and finally, provides a measure of the erosion potential for the ecosystem. Remote sensing presents a possible method for measuring dry residue. However, current satellites have had limited application due to the coarse spatial scales (relative to the patch dynamics) and insensitivity of the spectral coverage to resolve dry plant material. Several hypotheses for measuring the biochemical constituents of dry plant material, particularly cellulose and lignin, using high spectral resolution sensors were proposed. The use of Airborne Visible/Infrared Imaging Spectrometers (AVIRIS) to measure dry plant residues over an oak savannah on the eastern slopes of the Coast Range in central California was investigated and it was asked what spatial and spectral resolutions are needed to quantitatively measure dry plant biomass in this ecosystem.

  19. Investigation of enrofloxacin residues in broiler tissues using ELISA and LC-MS/MS.

    PubMed

    Panzenhagen, Pedro Henrique N; Aguiar, Waldemir S; Gouvêa, Raquel; de Oliveira, Andréa M G; Barreto, Fabiano; Pereira, Virgínia L A; Aquino, Maria Helena C

    2016-01-01

    This study investigated the efficiency of an enrofloxacin ELISA test kit to detect the presence of enrofloxacin residues in broiler tissues compared with LC-MS/MS. Broiler tissues from 72 samples consisting of 60 breast muscle, six pools of livers (500 g each) and six pools of kidneys (500 g each) were obtained from six different slaughterhouses. Breast muscle from 10 carcasses and pools of livers and kidneys from approximately 200 carcasses of the same flock were collected from each slaughterhouse. ELISA and HPLC were used to identify and quantify the contamination of the samples with enrofloxacin. A total of 72% of the analysed samples contained enrofloxacin residues detected by the ELISA and 22.2% were detected by LC-MS/MS. The mean values of enrofloxacin contamination found in chicken breast by ELISA and HPLC were 8.63 and 12.25 μg kg(-1), respectively. None of the samples exceeded the maximum limit of 100 μg kg(-1) by both methods set by the European Union as well as the Brazilian Agriculture Ministry. All positive samples for enrofloxacin residues detected by LC-MS/MS were also positive by ELISA. These data confirm the efficiency of the ELISA test, and suggest its use as a screening method for enrofloxacin residues in poultry tissues due to its quick results, low price and ease of applicability.

  20. Determination of quinolones and fluoroquinolones, tetracyclines and sulfonamides in bovine, swine and poultry liver using LC-MS/MS.

    PubMed

    Martins, Magda Targa; Barreto, Fabiano; Hoff, Rodrigo Barcelos; Jank, Louise; Arsand, Juliana Bazzan; Feijó, Tiago Correa; Schapoval, Elfrides Eva Scherman

    2015-01-01

    Antibacterials are widely used in veterinary medicine. Residues of these drugs can remain in food of animal origin, including bovine liver. This paper describes a fast and simple analytical method for the determination of quinolones and fluoroquinolones, tetracyclines and sulfonamides in bovine liver samples. Deuterated enrofloxacin, sulfapyridine and demeclocycline were used as internal standards. The homogenised liver samples were extracted with acidified acetonitrile. Steps of non-solid-phase extraction (SPE) clean-up and concentration were used in the presented method. The final extracts were analysed by sensitive and selective detection of all components in a single run using LC-MS/MS. Acceptable recoveries between 66% and 110% were obtained. Good linearity (r(2)) above 0.96, considering three different days, for all drugs was achieved in concentrations ranging from 0.0 to 2.0 × the maximum residue limit (MRL). Intraday precision with coefficient of variation (CV%) (n = 6) lower than 14.7% and inter-day precision lower than 18.8% in agreement with European Commission Decision 2002/657/EC were obtained in concentrations ranging from 0.5 to 1.5 MRL. Accuracy was between 86% and 110%. Limits of detection and quantitation, as well as decision limit (CCα) and detection capability (CCβ), were also evaluated.

  1. Lab-scale investigation on remediation of diesel-contaminated aquifer using microwave energy.

    PubMed

    Falciglia, Pietro P; Maddalena, Riccardo; Mancuso, Giuseppe; Messina, Valeria; Vagliasindi, Federico G A

    2016-02-01

    Aquifer contamination with diesel fuel is a worldwide environmental problem, and related available remediation technologies may not be adequately efficient, especially for the simultaneous treatment of both solid and water phases. In this paper, a lab-scale 2.45 GHz microwave (MW) treatment of an artificially diesel-contaminated aquifer was applied to investigate the effects of operating power (160, 350 and 500 W) and time on temperature profiles and contaminant removal from both solid and water phases. Results suggest that in diesel-contaminated aquifer MW remediation, power significantly influences the final reachable temperature and, consequently, contaminant removal kinetics. A maximum temperature of about 120 °C was reached at 500 W. Observed temperature values depended on the simultaneous irradiation of both aquifer grains and groundwater. In this case, solid phase heating is limited by the maximum temperature that interstitial water can reach before evaporation. A minimal residual diesel concentration of about 100 mg kg(-1) or 100 mg L(-1) was achieved by applying a power of 500 W for a time of 60 min for the solid or water phase, respectively. Measured residual TPH fractions showed that MW heating resulted in preferential effects of the removal of different TPH molecular weight fractions and that the evaporation-stripping phenomena plays a major role in final contaminant removal processes. The power low kinetic equation shows an excellent fit (r(2) > 0.993) with the solid phase residual concentration observed for all the powers investigated. A maximum diesel removal of 88 or 80% was observed for the MW treatment of the solid or water phase, respectively, highlighting the possibility to successfully and simultaneously remediate both the aquifer phases. Consequently, MW, compared to other biological or chemical-physical treatments, appears to be a better choice for the fast remediation of diesel-contaminated aquifers. Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. The presence of opportunistic pathogens, Legionella spp., L. pneumophila and Mycobacterium avium complex, in South Australian reuse water distribution pipelines.

    PubMed

    Whiley, H; Keegan, A; Fallowfield, H; Bentham, R

    2015-06-01

    Water reuse has become increasingly important for sustainable water management. Currently, its application is primarily constrained by the potential health risks. Presently there is limited knowledge regarding the presence and fate of opportunistic pathogens along reuse water distribution pipelines. In this study opportunistic human pathogens Legionella spp., L. pneumophila and Mycobacterium avium complex were detected using real-time polymerase chain reaction along two South Australian reuse water distribution pipelines at maximum concentrations of 10⁵, 10³ and 10⁵ copies/mL, respectively. During the summer period of sampling the concentration of all three organisms significantly increased (P < 0.05) along the pipeline, suggesting multiplication and hence viability. No seasonality in the decrease in chlorine residual along the pipelines was observed. This suggests that the combination of reduced chlorine residual and increased water temperature promoted the presence of these opportunistic pathogens.

  3. A topologically related singularity suggests a maximum preferred size for protein domains.

    PubMed

    Zbilut, Joseph P; Chua, Gek Huey; Krishnan, Arun; Bossa, Cecilia; Rother, Kristian; Webber, Charles L; Giuliani, Alessandro

    2007-02-15

    A variety of protein physicochemical as well as topological properties, demonstrate a scaling behavior relative to chain length. Many of the scalings can be modeled as a power law which is qualitatively similar across the examples. In this article, we suggest a rational explanation to these observations on the basis of both protein connectivity and hydrophobic constraints of residues compactness relative to surface volume. Unexpectedly, in an examination of these relationships, a singularity was shown to exist near 255-270 residues length, and may be associated with an upper limit for domain size. Evaluation of related G-factor data points to a wide range of conformational plasticity near this point. In addition to its theoretical importance, we show by an application of CASP experimental and predicted structures, that the scaling is a practical filter for protein structure prediction. 2006 Wiley-Liss, Inc.

  4. Elemental composition of game meat from Austria.

    PubMed

    Ertl, Kathrin; Kitzer, Roland; Goessler, Walter

    2016-06-01

    Concentrations of 26 elements (B, Na, Mg, P, S, K, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Mo, Cd, Sb, Ba, Hg, Pb, U) in wild game meat from Austria were analysed using an inductively coupled plasma mass spectrometer. All investigated animals were culled during the hunting season 2012/2013, including 10 chamois (Rupicapra rupicapra), 9 hare (Lepus europaeus), 10 pheasant (Phasianus colchicus), 10 red deer (Cervus elaphus), 12 roe deer (Capreolus capreolus) and 10 wild boar (Sus scrofa). In 19 out of 61 meat samples lead concentrations were higher than 0.1 mg/kg, the maximum limit in meat as set by the European Commission (Regulation EC No 1881/2006), which is most likely caused by ammunition residues. Especially, pellet shot animals and chamois show a high risk for lead contamination. Despite ammunition residues all investigated muscle samples show no further health risk with respect to metal contamination.

  5. Food safety in Thailand 2: Pesticide residues found in Chinese kale (Brassica oleracea), a commonly consumed vegetable in Asian countries.

    PubMed

    Wanwimolruk, Sompon; Kanchanamayoon, Onnicha; Phopin, Kamonrat; Prachayasittikul, Virapong

    2015-11-01

    There is increasing public concern over human health risks associated with extensive use of pesticides in agriculture. Regulation of pesticide maximum residue limits (MRLs) in food commodities is established in many developed countries. For Thailand, this regulation exists in law but is not fully enforced. Therefore, pesticide residues in vegetables and fruits have not been well monitored. This study investigated the pesticide residues in Chinese kale, a commonly eaten vegetable among Asians. The Chinese kale samples (N = 117) were purchased from markets in Nakhon Pathom Province, Thailand, and analyzed for the content of 28 pesticides. Analysis was performed by the multiresidual extraction followed by GC-MS/MS. Of pesticides investigated, 12 pesticides were detected in 85% of the Chinese kale samples. Although carbaryl, deltamethrin, diazinon, fenvalerate and malathion were found in some samples, their levels were lower than their MRLs. However, in 34 samples tested, either carbofuran, chlorpyrifos, chlorothalonil, cypermethrin, dimethoate, metalaxyl or profenofos was detected exceeding their MRLs. This represents a 29% rate of pesticide detection above the MRL; a rate much higher than in developed countries. Washing vegetables under running water significantly reduced (p < 0.05) profenofos residues by 55%. The running water method did not significantly decrease cypermethrin residues in the samples but washing with vinegar did. Our research suggests that routine monitoring of pesticide residues is necessary to reduce the public health risks associated with eating contaminated vegetables. Washing vegetables before consumption is advisable as this helps to reduce the level of pesticide residues in our daily intake. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Bioefficacy evaluation and dissipation pattern of nanoformulation versus commercial formulation of pyridalyl in tomato (Solanum lycopersicum).

    PubMed

    Saini, Priya; Gopal, Madhuban; Kumar, Rajesh; Gogoi, Robin; Srivastava, Chitra

    2015-08-01

    A study was undertaken to evaluate the decline of the residues of pyridalyl in tomatoes grown in two different cultivation systems: open field (conventional cultivation) and net house (pot experiment). Field experiment was conducted with commercial (10 EC) and nanoformulation of pyridalyl on tomato crop. Tomato plants were subjected to pesticide spray, when fruits were close to ripeness. Fruit samples were taken periodically and cleaned up using QuEChERS methodology, and the residue of pyridalyl was analyzed by ultrahigh-performance liquid chromatography (UHPLC). It dissipated in tomato fruit following the first-order kinetics. In field, average initial deposit of pyridalyl in tomato was observed to be 0.222 and 0.371 μg g(-1) at recommended and double the recommended application rate, respectively, using nanoformulation while it was 0.223 and 0.393 μg g(-1) on using commercial formulation, respectively. The half-life (t1/2) value of nanopyridalyl in tomato fruit was 2.8 and 3.2 days while for commercial formulation, it was 2.5 and 2.6 days for recommended and double the recommended dose, respectively. In India, maximum residue limit (MRL) on tomato has not been fixed for pyridalyl but its residues were always below European MRLs (5 μg g(-1)) on tomato at both application rates. The results of terminal residue showed that pyridalyl residues were below the available MRL. Low residues in tomatoes suggested that this pesticide is safe to use under the recommended dosage. No statistical differences were observed between the cultivation systems in relation to the residue levels of pyridalyl.

  7. Deposition and residues of azoxystrobin and imidacloprid on greenhouse lettuce with implications for human consumption.

    PubMed

    Itoiz, Eva Sevigné; Fantke, Peter; Juraske, Ronnie; Kounina, Anna; Vallejo, Assumpció Antón

    2012-11-01

    Lettuce greenhouse experiments were carried out from March to June 2011 in order to analyze how pesticides behave from the time of application until their intake via human consumption taking into account the primary distribution of pesticides, field dissipation, and post-harvest processing. In addition, experimental conditions were used to evaluate a new dynamic plant uptake model comparing its results with the experimentally derived residues. One application of imidacloprid and two of azoxystrobin were conducted. For evaluating primary pesticide distribution, two approaches based on leaf area index and vegetation cover were used and results were compared with those obtained from a tracer test. High influence of lettuce density, growth stage and type of sprayer was observed in primary distribution showing that low densities or early growth stages implied high losses of pesticides on soil. Washed and unwashed samples of lettuce were taken and analyzed from application to harvest to evaluate removal of pesticides by food processing. Results show that residues found on the Spanish preharvest interval days were in all cases below officially set maximum residue limits, although it was observed that time between application and harvest is as important for residues as application amounts. An overall reduction of 40-60% of pesticides residues was obtained from washing lettuce. Experimentally derived residues were compared with modeled residues and deviate from 1.2 to 1.4 for imidacloprid and azoxystrobin, respectively, presenting good model predictions. Resulting human intake fractions range from 0.045 kg(intake) kg(applied)(-1) for imidacloprid to 0.14 kg(intake) kg(applied)(-1) for azoxystrobin. Copyright © 2012 Elsevier Ltd. All rights reserved.

  8. Successive monitoring surveys of selected banned and restricted pesticide residues in vegetables from the northwest region of China from 2011 to 2013.

    PubMed

    Yu, Yan; Hu, Senke; Yang, Yuxuan; Zhao, Xiaodan; Xue, Jianjun; Zhang, Jinghua; Gao, Song; Yang, Aimin

    2017-08-02

    A wide range of pesticides is applied for crop protection in vegetable cultivation in China. Regulation of pesticide maximum residue limits (MRLs) in vegetables is established but not fully enforced. And pesticide residues in vegetables were not well monitored. This study conducted the monitoring surveys from 2011 to 2013 to investigate the pesticides in vegetables in the northwest region of China. A multi-residue gas chromatography/mass spectrometry method (GC/MS) was used in determination of pesticides in vegetable samples. The χ 2 test was used to compare the concentration of pesticide residues. A total of 32 pesticide residues were detected in 518 samples from 20 types of vegetables in this study. 7.7% of the detected pesticide residues exceeded the MRLs. The percentages of residues that exceeded the MRLs for leafy, melon and fruit, and root vegetables were 11.2%, 5.1%, and 1.6%, respectively. There was no seasonal difference in the proportion of samples that exceeded the MRLs in different vegetables. A total of 84.3% (27/32) pesticides were detected at concentrations that exceeded MRLs. And of the 27 pesticides that exceeded the MRLs, 11 (40.7%) were banned for use in agriculture. The most frequently detected pesticides were Malathion (9.4%), Dichlorvos (8.7%), and Dimethoate (8.1%). The observed high rate of pesticides detected and high incidence of pesticide detection exceeding their MRLs in the commonly consumed vegetables indicated that the Good Agricultural Practices (GAP) may not be well followed. The management of pesticide use and control should be improved. Well-developed training programs should be initiated to improve pesticide application knowledge for farmers.

  9. Development and validation of an ultra performance liquid chromatography Q-Exactive Orbitrap mass spectrometry for the determination of fipronil and its metabolites in tea and chrysanthemum.

    PubMed

    Chen, Hongping; Gao, Guanwei; Liu, Pingxiang; Pan, Meiling; Chai, Yunfeng; Liu, Xin; Lu, Chengyin

    2018-04-25

    A fast, sensitive and reliable method for the determination of fipronil and its metabolites in tea and chrysanthemum was developed using a modified QuEChERS technique and an ultra performance liquid chromatography Q-Exactive Orbitrap mass spectrometry. The mixture of adsorbents containing primary secondary amine (PSA), octadecylsilane (C 18 ) and carbon nanotubes (CNTs), was used as QuEChERS adsorbents. The use of mass resolution at 70000 full width at half maximum (FWHM) and narrow mass windows at 5 ppm achieved high selectivity and repeatability. Satisfactory linearity with correlative coefficient (R 2 ) higher than 0.996 was achieved for all compounds. Recoveries at three levels (2, 10 and 50 μg kg -1 ) ranged from 86% to 112%, while the intra- and inter-day accuracies were less than 15%. Limits of quantification for fipronil and its metabolites were 2 μg kg -1 , which fulfils the requirement of maximum residue limits formulated by European Union and Japan. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Screening of antibiotics and chemical analysis of penicillin residue in fresh milk and traditional dairy products in Oyo state, Nigeria

    PubMed Central

    Olatoye, Isaac Olufemi; Daniel, Oluwayemisi Folashade; Ishola, Sunday Ayobami

    2016-01-01

    Background and Aim: There are global public health and economic concerns on chemical residues in food of animal origin. The use of antibiotics in dairy cattle for the treatment of diseases such as mastitis has contributed to the presence of residues in dairy products. Penicillin residues as low as 1 ppb can lead to allergic reactions and shift of resistance patterns in microbial population as well as interfere with the processing of several dairy products. Antibiotic monitoring is an essential quality control measure in safe milk production. This study was aimed at determining antibiotic residue contamination and the level of penicillin in dairy products from Fulani cattle herds in Oyo State. Materials and Methods: The presence of antibiotic residues in 328 samples of fresh milk, 180 local cheese (wara), and 90 fermented milk (nono) from Southwest, Nigeria were determined using Premi® test kit (R-Biopharm AG, Germany) followed by high-performance liquid chromatography analysis of penicillin-G residue. Results: Antibiotic residues were obtained in 40.8%, 24.4% and 62.3% fresh milk, wara and nono, respectively. Penicillin-G residue was also detected in 41.1% fresh milk, 40.2% nono and 24.4% wara at mean concentrations of 15.22±0.61, 8.24±0.50 and 7.6±0.60 μg/L with 39.3%, 36.7% and 21.1%, respectively, containing penicillin residue above recommended Codex maximum residue limit (MRL) of 5 μg/L in dairy. There was no significant difference between the mean penicillin residues in all the dairy products in this study. Conclusion: The results are of food safety concern since the bulk of the samples and substantial quantities of dairy products in Oyo state contained violative levels of antibiotic residues including penicillin residues in concentrations above the MRL. This could be due to indiscriminate and unregulated administration of antibiotics to dairy cattle. Regulatory control of antibiotic use, rapid screening of milk and dairy farmers’ extension education on alternatives to antibiotic prophylaxis, veterinary prescriptions and withdrawal periods are recommended to prevent residues. PMID:27733794

  11. Determination of the Ability to Measure Traces of Water in Dehydrated Residues of Waste Water by IR Diffuse Reflectance Spectra

    NASA Astrophysics Data System (ADS)

    Pratsenka, S. V.; Voropai, E. S.; Belkin, V. G.

    2018-01-01

    Rapid measurement of the moisture content of dehydrated residues is a critical problem, the solution of which will increase the efficiency of treatment facilities and optimize the process of applying flocculants. The ability to determine the moisture content of dehydrated residues using a meter operating on the IR reflectance principle was confirmed experimentally. The most suitable interference filters were selected based on an analysis of the obtained diffuse reflectance spectrum of the dehydrated residue in the range 1.0-2.7 μm. Calibration curves were constructed and compared for each filter set. A measuring filter with a transmittance maximum at 1.19 μm and a reference filter with a maximum at 1.3 μm gave the best agreement with the laboratory measurements.

  12. An electrochemical magneto immunosensor (EMIS) for the determination of paraquat residues in potato samples.

    PubMed

    Garcia-Febrero, Raul; Valera, Enrique; Muriano, Alejandro; Pividori, M-Isabel; Sanchez-Baeza, Francisco; Marco, M-Pilar

    2013-09-01

    An electrochemical magneto immunosensor for the detection of low concentrations of paraquat (PQ) in food samples has been developed and its performance evaluated in a complex sample such as potato extracts. The immunosensor presented uses immunoreagents specifically developed for the recognition of paraquat, a magnetic graphite-epoxy composite (m-GEC) electrode and biofunctionalized magnetic micro-particles (PQ1-BSAMP) that allow reduction of the potential interferences caused by the matrix components. The amperometric signal is provided by an enzymatic probe prepared by covalently linking an enzyme to the specific antibodies (Ab198-cc-HRP). The use of hydroquinone, as mediator, allows recording of the signal at a low potential, which also contributes to reducing the background noise potentially caused by the sample matrix. The immunocomplexes formed on top of the modified MP are easily captured by the m-GEC, which acts simultaneously as transducer. PQ can be detected at concentrations as low as 0.18 ± 0.09 μg L(-1). Combined with an efficient extraction procedure, PQ residues can be directly detected and accurately quantified in potato extracts without additional clean-up or purification steps, with a limit of detection (90% of the maximum signal) of 2.18 ± 2.08 μg kg(-1), far below the maximum residue level (20 μg kg(-1)) established by the EC. The immunosensor presented here is suitable for on-site analysis. Combined with the use of magnetic racks, multiple samples can be run simultaneously in a reasonable time.

  13. Evaluation of a Microbiological Multi-Residue System on the detection of antibacterial substances in ewe milk.

    PubMed

    Althaus, Rafael; Berruga, Maria Isabel; Montero, Ana; Roca, Marta; Molina, Maria Pilar

    2009-01-19

    To protect both, public health and the dairy industry, from the presence of antibiotic residues in milk, control programmes have been established, which include the needed screening tests. This work focuses on the application of a Microbiological Multi-Residue System in ewe milk, a method based on the use of six different plates, each seeded with one of the following bacteria: Geobacillus stearothermophilus var. calidolactis (beta-lactams), Bacillus subtilis at pH 8.0 (aminoglycosides), Kocuria rhizophila (macrolides), Escherichia coli (quinolones), B. cereus (tetracyclines) and B. subtilis at pH 7.0 (sulphonamides), respectively. Twenty-three antimicrobial substances were analysed and a logistic regression was established for each substance assayed to relate the antibiotic concentration and the zone of microbial growth inhibition. Great linearity in the response was observed (regression coefficients of over 0.97). This fact suggests the possibility of establishing a decision level of antibiotic concentrations near to the Maximum Residue Limits (MRL). Zones of inhibition were suggested as proposed action levels for the different antimicrobial groups (diameters of inhibition of 18 mm for the aminoglycoside, beta-lactam and sulphonamide plates; 19 mm for the tetracycline plate, 21 mm for the macrolide plate, and 24 mm for the quinolone plate). Specificity and cross-reactivity were also assayed.

  14. Analysis of pesticide residues in strawberries and soils by GC-MS/MS, LC-MS/MS and two-dimensional GC-time-of-flight MS comparing organic and integrated pest management farming.

    PubMed

    Fernandes, Virgínia C; Lehotay, Steven J; Geis-Asteggiante, Lucía; Kwon, Hyeyoung; Mol, Hans G J; van der Kamp, Henk; Mateus, Nuno; Domingues, Valentina F; Delerue-Matos, Cristina

    2014-01-01

    This study analysed 22 strawberry and soil samples after their collection over the course of 2 years to compare the residue profiles from organic farming with integrated pest management practices in Portugal. For sample preparation, we used the citrate-buffered version of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. We applied three different methods for analysis: (1) 27 pesticides were targeted using LC-MS/MS; (2) 143 were targeted using low pressure GC-tandem mass spectrometry (LP-GC-MS/MS); and (3) more than 600 pesticides were screened in a targeted and untargeted approach using comprehensive, two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOF-MS). Comparison was made of the analyses using the different methods for the shared samples. The results were similar, thereby providing satisfactory confirmation of both similarly positive and negative findings. No pesticides were found in the organic-farmed samples. In samples from integrated pest management practices, nine pesticides were determined and confirmed to be present, ranging from 2 µg kg(-1) for fluazifop-p-butyl to 50 µg kg(-1) for fenpropathrin. Concentrations of residues in strawberries were less than European maximum residue limits.

  15. Hands-Off and Hands-On Casting Consistency of Amputee below Knee Sockets Using Magnetic Resonance Imaging

    PubMed Central

    Rowe, Philip

    2013-01-01

    Residual limb shape capturing (Casting) consistency has a great influence on the quality of socket fit. Magnetic Resonance Imaging was used to establish a reliable reference grid for intercast and intracast shape and volume consistency of two common casting methods, Hands-off and Hands-on. Residual limbs were cast for twelve people with a unilateral below knee amputation and scanned twice for each casting concept. Subsequently, all four volume images of each amputee were semiautomatically segmented and registered to a common coordinate system using the tibia and then the shape and volume differences were calculated. The results show that both casting methods have intra cast volume consistency and there is no significant volume difference between the two methods. Inter- and intracast mean volume differences were not clinically significant based on the volume of one sock criteria. Neither the Hands-off nor the Hands-on method resulted in a consistent residual limb shape as the coefficient of variation of shape differences was high. The resultant shape of the residual limb in the Hands-off casting was variable but the differences were not clinically significant. For the Hands-on casting, shape differences were equal to the maximum acceptable limit for a poor socket fit. PMID:24348164

  16. Residue analysis and risk assessment of tebuconazole in jujube (Ziziphus jujuba Mill).

    PubMed

    You, Xiangwei; Li, Yiqiang; Wang, Xiuguo; Xu, Jinli; Zheng, Xiao; Sui, Chengcheng

    2017-07-01

    In this study, a sensitive and reliable analytical method, based on a modified Quick, Easy, Cheap, Effective, Rugged and Safe procedure, was established for determination of tebuconazole in jujube. After extraction with acetonitrile, the samples were cleaned up by dispersive solid-phase extraction with primary secondary amine, and determined by high-performance liquid chromatography tandem mass spectrometry. At fortification levels of 0.01, 0.1 and 2.0 mg kg -1 , the average recoveries of tebuconazole in jujube were in the range 97.6-101.9%, with relative standard deviations of 1.5-3.5%. The dissipation and residual levels of tebuconazole in jujube under field conditions were investigated. Tebuconazole dissipated relatively slowly in jujube, with a half-life of 33.0 days. The terminal residue experiments of tebuconazole in jujube were conducted in four locations in China and the risk was evaluated using risk quotients (RQ). RQ values were found to be significantly lower than RQ = 1, indicating that the risk to human health of using the recommended doses of tebuconazole in jujube was not significant. This study could provide guidance for the safe and reasonable use of tebuconazole in jujube and serve as a reference for the establishment of limit of maximum residue in China. Copyright © 2016 John Wiley & Sons, Ltd.

  17. Influence of erroneous patient records on population pharmacokinetic modeling and individual bayesian estimation.

    PubMed

    van der Meer, Aize Franciscus; Touw, Daniël J; Marcus, Marco A E; Neef, Cornelis; Proost, Johannes H

    2012-10-01

    Observational data sets can be used for population pharmacokinetic (PK) modeling. However, these data sets are generally less precisely recorded than experimental data sets. This article aims to investigate the influence of erroneous records on population PK modeling and individual maximum a posteriori Bayesian (MAPB) estimation. A total of 1123 patient records of neonates who were administered vancomycin were used for population PK modeling by iterative 2-stage Bayesian (ITSB) analysis. Cut-off values for weighted residuals were tested for exclusion of records from the analysis. A simulation study was performed to assess the influence of erroneous records on population modeling and individual MAPB estimation. Also the cut-off values for weighted residuals were tested in the simulation study. Errors in registration have limited the influence on outcomes of population PK modeling but can have detrimental effects on individual MAPB estimation. A population PK model created from a data set with many registration errors has little influence on subsequent MAPB estimates for precisely recorded data. A weighted residual value of 2 for concentration measurements has good discriminative power for identification of erroneous records. ITSB analysis and its individual estimates are hardly affected by most registration errors. Large registration errors can be detected by weighted residuals of concentration.

  18. Hands-off and hands-on casting consistency of amputee below knee sockets using magnetic resonance imaging.

    PubMed

    Safari, Mohammad Reza; Rowe, Philip; McFadyen, Angus; Buis, Arjan

    2013-01-01

    Residual limb shape capturing (Casting) consistency has a great influence on the quality of socket fit. Magnetic Resonance Imaging was used to establish a reliable reference grid for intercast and intracast shape and volume consistency of two common casting methods, Hands-off and Hands-on. Residual limbs were cast for twelve people with a unilateral below knee amputation and scanned twice for each casting concept. Subsequently, all four volume images of each amputee were semiautomatically segmented and registered to a common coordinate system using the tibia and then the shape and volume differences were calculated. The results show that both casting methods have intra cast volume consistency and there is no significant volume difference between the two methods. Inter- and intracast mean volume differences were not clinically significant based on the volume of one sock criteria. Neither the Hands-off nor the Hands-on method resulted in a consistent residual limb shape as the coefficient of variation of shape differences was high. The resultant shape of the residual limb in the Hands-off casting was variable but the differences were not clinically significant. For the Hands-on casting, shape differences were equal to the maximum acceptable limit for a poor socket fit.

  19. Analytical Confirmation of Various Herbicides in Drinking Water Resources in Sugarcane Production Regions of Guangxi, China.

    PubMed

    Li, Honghong; Feng, Yujie; Li, Xuesheng; Zeng, Dongqiang

    2018-06-01

    This work investigated drinking water contamination by 11 commonly used herbicides in sugarcane production areas in Guangxi, China. The work developed an analytical method for determination of these herbicides in environmental waters. This work studied herbicide residues in drinking water in Guangxi, China. The maximum residues and percent of detects were: (0.091 µg/L, 29.2%, atrazine), (0.018 µg/L, 8.3%, ametryne), (0.188 µg/L, 8.3%, aetolaehlor), (0.139 µg/L, 4%, simazine), (0.585 µg/L, 62.5%, atrazine), (0.311 µg/L, 33.3%, acetochlor), (0.341 µg/L, 58.3%, ametryne), (1.312 µg/L, 29.2%, metolachlor), (0.088 µg/L, 4.2%, alachlor), (0.127 µg/L, 14.3%, atrazine), and (0.453 µg/L, 7.1%, metolachlor), respectively. The results demonstrated that agricultural herbicides were detected in all water samples, including tap, surface and groundwater samples. Since the residues are generally below the safe limits established by the government authorities, the monitored 11 herbicides do not significantly affect the quality of the human environment. This work will provide scientific understanding of pesticide residues in drinking water standards in terms of its consistency with precautionary human health and environmental safety.

  20. Determination of anthelmintic drug residues in milk using ultra high performance liquid chromatography-tandem mass spectrometry with rapid polarity switching.

    PubMed

    Whelan, Michelle; Kinsella, Brian; Furey, Ambrose; Moloney, Mary; Cantwell, Helen; Lehotay, Steven J; Danaher, Martin

    2010-07-02

    A new UHPLC-MS/MS (ultra high performance liquid chromatography coupled to tandem mass spectrometry) method was developed and validated to detect 38 anthelmintic drug residues, consisting of benzimidazoles, avermectins and flukicides. A modified QuEChERS-type extraction method was developed with an added concentration step to detect most of the analytes at <1 microg kg(-1) levels in milk. Anthelmintic residues were extracted into acetonitrile using magnesium sulphate and sodium chloride to induce liquid-liquid partitioning followed by dispersive solid phase extraction for cleanup. The extract was concentrated into dimethyl sulphoxide, which was used as a keeper to ensure analytes remain in solution. Using rapid polarity switching in electrospray ionisation, a single injection was capable of detecting both positively and negatively charged ions in a 13 min run time. The method was validated at two levels: the unapproved use level and at the maximum residue level (MRL) according to Commission Decision (CD) 2002/657/EC criteria. The decision limit (CCalpha) of the method was in the range of 0.14-1.9 and 11-123 microg kg(-1) for drugs validated at unapproved and MRL levels, respectively. The performance of the method was successfully verified for benzimidazoles and levamisole by participating in a proficiency study.

  1. Accumulation of steroid hormones in soil and its adjacent aquatic environment from a typical intensive vegetable cultivation of North China.

    PubMed

    Zhang, Feng-Song; Xie, Yun-Feng; Li, Xue-Wen; Wang, Dai-Yi; Yang, Lin-Sheng; Nie, Zhi-Qiang

    2015-12-15

    Steroid hormones released from manure agricultural application are a matter of global concern. The residual levels of steroid hormones were studied in a typical intensive vegetable cultivation area in northeast China, with a long history of heavy manure application. Seven steroids (estrone, 17α-estradiol, 17β-estradiol, estriol, testosterone, androstendione and progesterone) were analyzed from soil sampled from vegetable greenhouses, from sediments and water from the adjacent drainage ditch and from the groundwater. The results showed that target steroids were detected in the soil samples, with detection frequencies varying from 3.13 to 100%. The steroid concentrations varied substantially in soils, ranging from below the detection limit to 109.7μg·kg(-1). Three steroids-progesterone, androstendione and estrone-were found to have relatively high residue concentrations in soil, with maximum concentrations of 109.7, 9.83 and 13.30μg·kg(-1), respectively. In adjacent groundwater, all the steroids, with the exception of estrone, were detected in one or more of the 13 groundwater samples. The concentrations of steroids in groundwater ranged from below the method detection limit to 2.38ng·L(-1). Six of the seven (excluding androstendione) were detected in drainage ditch water samples, with concentrations ranging from below the detection limit to 14ng·L(-1). Progesterone, androstendione and estrone accumulated relatively easily in soils; their concentrations in groundwater were lower than those of other steroids. The concentrations of testosterone and estriol were relatively low in soil, while in groundwater were higher than those of other steroids. The residual levels of steroids in soil and groundwater showed a clear spatial variation in the study area. The residual levels of steroid hormones in soil varied substantially between differently planted greenhouses. Copyright © 2015. Published by Elsevier B.V.

  2. Organochlorine insecticide residues in the free-tailed bat (Tadarida brasiliensis) at Bracken Cave, Texas

    USGS Publications Warehouse

    Clark, D.R.; Martin, C.O.; Swineford, D.M.

    1975-01-01

    Fifty-nine free-tailed bats (Tadarida brasiliensis mexicana ) were collected at Bracken Cave, Texas, and analyzed for organochlorine insecticides and polychlorinated biphenyls (PCBs). Residues of DDE in the brain were greater in 12 young collected from the floor than in 15 young taken from the ceiling, but food deprivation, not higher residues in the brain, apparently caused young to fall....Among 18 pregnant females, residues of DDE and DDT were highest in yearlings. The first lactation by yearlings caused their residue loads to drop sharply. Thereafter, increasing age was accompanied by increasing residues but amounts generally did not exceed those in yearlings.....Residue levels in embryos were a function both of levels in the female parent and degree of embryonic development. Residues accumulated rapidly in nursing young, and lactating females may excrete from 1.3 to 16.2 (mean = 4.3) micrograms of DDE in milk per day. Maximum individual residue loads may be attained toward the end of nursing, and mobilization of these residues during southward migration may subject Bracken Cave free-tails to maximum lifetime residues in the brain....Comparison of our data with residue data for the free-tail population at Eagle Creek Cave (Arizona) in 1970 produced the following conclusions: ( 1) residues of DDE appeared similar in pregnant females, embryos, lactating females, and fallen young for the two populations; (2) residues of DDT and dieldrin appeared greater in pregnant females at Bracken Cave; (3) DDE and DDT occurred at greater levels in guano samples from Bracken Cave. On this basis, the population decline observed at Eagle Creek Cave between 1963 and 1969 does not appear to be related to the residues observed in the 1970 samples taken from that cave.

  3. 21 CFR 172.882 - Synthetic isoparaffinic petroleum hydrocarbons.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... American Society for Testing Materials, 100 Barr Harbor Dr., West Conshohocken, Philadelphia, PA 19428-2959.../code_of_federal_regulations/ibr_locations.html. Ultraviolet absorbance: 260-319 millimicrons—1.5 maximum. 320-329 millimicrons—0.08 maximum. 330-350 millimicrons—0.05 maximum. Nonvolatile residual: 0.002...

  4. Determining crop residue type and class using satellite acquired data. M.S. Thesis Progress Report, Jun. 1990

    NASA Technical Reports Server (NTRS)

    Zhuang, Xin

    1990-01-01

    LANDSAT Thematic Mapper (TM) data for March 23, 1987 with accompanying ground truth data for the study area in Miami County, IN were used to determine crop residue type and class. Principle components and spectral ratioing transformations were applied to the LANDSAT TM data. One graphic information system (GIS) layer of land ownership was added to each original image as the eighth band of data in an attempt to improve classification. Maximum likelihood, minimum distance, and neural networks were used to classify the original, transformed, and GIS-enhanced remotely sensed data. Crop residues could be separated from one another and from bare soil and other biomass. Two types of crop residue and four classes were identified from each LANDSAT TM image. The maximum likelihood classifier performed the best classification for each original image without need of any transformation. The neural network classifier was able to improve the classification by incorporating a GIS-layer of land ownership as an eighth band of data. The maximum likelihood classifier was unable to consider this eighth band of data and thus, its results could not be improved by its consideration.

  5. Health risk for children and adults consuming apples with pesticide residue.

    PubMed

    Lozowicka, Bozena

    2015-01-01

    The presence of pesticide residues in apples raises serious health concerns, especially when the fresh fruits are consumed by children, particularly vulnerable to the pesticide hazards. This study demonstrates the results from nine years of investigation (2005-2013) of 696 samples of Polish apples for 182 pesticides using gas and liquid chromatography and spectrophotometric techniques. Only 33.5% of the samples did not contain residues above the limit of detection. In 66.5% of the samples, 34 pesticides were detected, of which maximum residue level (MRL) was exceeded in 3%. Multiple residues were present in 35% of the samples with two to six pesticides, and one sample contained seven compounds. A study of the health risk for children, adults and the general population consuming apples with these pesticides was performed. The pesticide residue data have been combined with the consumption of apples in the 97.5 percentile and the mean diet. A deterministic model was used to assess the chronic and acute exposures that are based on the average and high concentrations of residues. Additionally, the "worst-case scenario" and "optimistic case scenario" were used to assess the chronic risk. In certain cases, the total dietary pesticide intake calculated from the residue levels observed in apples exceeds the toxicological criteria. Children were the group most exposed to the pesticides, and the greatest short-term hazard stemmed from flusilazole at 624%, dimethoate at 312%, tebuconazole at 173%, and chlorpyrifos methyl and captan with 104% Acute Reference Dose (ARfD) each. In the cumulative chronic exposure, among the 17 groups of compounds studied, organophosphate insecticides constituted 99% acceptable daily intake (ADI). The results indicate that the occurrence of pesticide residues in apples could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring and tighter regulation of pesticide residues is recommended. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. [Radioactive cesium analysis in radiation-tainted beef by gamma-ray spectrometry with germanium semiconductor detector].

    PubMed

    Minatani, Tomiaki; Nagai, Hiroyuki; Nakamura, Masashi; Otsuka, Kimihito; Sakai, Yoshimichi

    2012-01-01

    The detection limit and precision of radioactive cesium measurement in beef by gamma-ray spectrometry with a germanium semiconductor detector were evaluated. Measurement for 2,000 seconds using a U-8 container (100 mL) provided a detection limit of radioactive cesium (the sum of 134Cs and 137Cs) of around 20 Bq/kg. The 99% confidence interval of the measurement of provisional maximum residue limit level (491 Bq/kg) samples ranged from 447 to 535 Bq/kg. Beef is heterogeneous, containing muscle and complex fat layers. Depending on the sampled parts, the measurement value is variable. It was found that radioactive cesium content of the muscle layer was clearly different from that of fat, and slight differences were observed among parts of the sample (SD=16.9 Bq/kg), even though the same region (neck block) of beef sample was analyzed.

  7. Rapid detection and quantification of 2,4-dichlorophenoxyacetic acid in milk using molecularly imprinted polymers-surface-enhanced Raman spectroscopy.

    PubMed

    Hua, Marti Z; Feng, Shaolong; Wang, Shuo; Lu, Xiaonan

    2018-08-30

    We report the development of a molecularly imprinted polymers-surface-enhanced Raman spectroscopy (MIPs-SERS) method for rapid detection and quantification of a herbicide residue 2,4-dichlorophenoxyacetic acid (2,4-D) in milk. MIPs were synthesized via bulk polymerization and utilized as solid phase extraction sorbent to selectively extract and enrich 2,4-D from milk. Silver nanoparticles were synthesized to facilitate the collection of SERS spectra of the extracts. Based on the characteristic band intensity of 2,4-D (391 cm -1 ), the limit of detection was 0.006 ppm and the limit of quantification was 0.008 ppm. A simple logarithmic working range (0.01-1 ppm) was established, satisfying the sensitivity requirement referring to the maximum residue level of 2,4-D in milk in both Europe and North America. The overall test of 2,4-D for each milk sample required only 20 min including sample preparation. This MIPs-SERS method has potential for practical applications in detecting 2,4-D in agri-foods. Copyright © 2018 Elsevier Ltd. All rights reserved.

  8. Ractopamine analysis in pig kidney, liver and lungs: A validation of the method scope extension using QuEChERS as a sample preparation step.

    PubMed

    Feddern, Vivian; Aroeira, Carolina Naves; Molognoni, Luciano; Gressler, Vanessa; Daguer, Heitor; Dalla Costa, Osmar Antonio; Castillo, Carmen Josefina Contreras; de Lima, Gustavo Julio Mello Monteiro

    2018-05-23

    Ractopamine has been allowed by some countries as a repartitioning additive in pig diet, since it promotes protein synthesis and fat lipolysis. Most regulatory agencies only propose the ractopamine assessment in meat, kidney, liver and fat. Aiming at contributing to the scarcity data regarding this analyte in pig lungs, we extended the scope of a LC-MS method to evaluate pig offals. Homogenized tissue samples were extracted by a QuEChERS procedure; following by clean up steps and further tandem mass spectrometry determination. Method performance was evaluated through specificity, recovery, linearity, reproducibility, repeatability, decision limit (CC α ), and detection capability (CC β ), in accordance to the Commission Decision 2002/657/EC. Regression coefficients (R 2 ) between 0.994 and 0.999 were achieved for kidney, liver and lungs. Recoveries ranged from 92.0 to 127%. CC α and CC β values ranged from 3.65 to 4.86 μg kg -1 , and from 6.27 to 7.21 μg kg -1 , respectively. These values were under the maximum residue limits suggested by Codex Alimentarius, which are 90 and 40 μg kg -1 for kidney and liver, respectively. When applied to real samples up to 22.5, 92 and 1003 μg kg -1 of ractopamine residues were detected in pig liver, kidney and lungs, respectively. The results allowed concluding that the proposed analytical method is capable to detect ractopamine residues in all evaluated matrices. Therefore, it can be successfully applied and used as a routine method in laboratories of residue analysis. Copyright © 2018. Published by Elsevier B.V.

  9. Evaluation of Methane from Sisal Leaf Residue and Palash Leaf Litter

    NASA Astrophysics Data System (ADS)

    Arisutha, S.; Baredar, P.; Deshpande, D. M.; Suresh, S.

    2014-12-01

    The aim of this study is to evaluate methane production from sisal leaf residue and palash leaf litter mixed with different bulky materials such as vegetable market waste, hostel kitchen waste and digested biogas slurry in a laboratory scale anaerobic reactor. The mixture was prepared with 1:1 proportion. Maximum methane content of 320 ml/day was observed in the case of sisal leaf residue mixed with vegetable market waste as the feed. Methane content was minimum (47 ml/day), when palash leaf litter was used as feed. This was due to the increased content of lignin and polyphenol in the feedstock which were of complex structure and did not get degraded directly by microorganisms. Sisal leaf residue mixtures also showed highest content of volatile fatty acids (VFAs) as compared to palash leaf litter mixtures. It was observed that VFA concentration in the digester first increased, reached maximum (when pH was minimum) and then decreased.

  10. 49 CFR 173.417 - Authorized fissile materials packages.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... for export and import shipments. (2) A residual “heel” of enriched solid uranium hexafluoride may be... “Heel” in a Specification 7A Cylinder) Maximum cylinder diameter Centimeters Inches Cylinder volume Liters Cubic feet Maximum Uranium 235-enrichment (weight)percent Maximum “Heel” weight per cylinder UF6...

  11. 49 CFR 173.417 - Authorized fissile materials packages.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... for export and import shipments. (2) A residual “heel” of enriched solid uranium hexafluoride may be... “Heel” in a Specification 7A Cylinder) Maximum cylinder diameter Centimeters Inches Cylinder volume Liters Cubic feet Maximum Uranium 235-enrichment (weight)percent Maximum “Heel” weight per cylinder UF6...

  12. Dynamic Response and Residual Helmet Liner Crush Using Cadaver Heads and Standard Headforms.

    PubMed

    Bonin, S J; Luck, J F; Bass, C R; Gardiner, J C; Onar-Thomas, A; Asfour, S S; Siegmund, G P

    2017-03-01

    Biomechanical headforms are used for helmet certification testing and reconstructing helmeted head impacts; however, their biofidelity and direct applicability to human head and helmet responses remain unclear. Dynamic responses of cadaver heads and three headforms and residual foam liner deformations were compared during motorcycle helmet impacts. Instrumented, helmeted heads/headforms were dropped onto the forehead region against an instrumented flat anvil at 75, 150, and 195 J. Helmets were CT scanned to quantify maximum liner crush depth and crush volume. General linear models were used to quantify the effect of head type and impact energy on linear acceleration, head injury criterion (HIC), force, maximum liner crush depth, and liner crush volume and regression models were used to quantify the relationship between acceleration and both maximum crush depth and crush volume. The cadaver heads generated larger peak accelerations than all three headforms, larger HICs than the International Organization for Standardization (ISO), larger forces than the Hybrid III and ISO, larger maximum crush depth than the ISO, and larger crush volumes than the DOT. These significant differences between the cadaver heads and headforms need to be accounted for when attempting to estimate an impact exposure using a helmet's residual crush depth or volume.

  13. Presence of pesticide residues on produce cultivated in Suriname.

    PubMed

    Abdoel Wahid, F; Wickliffe, J; Wilson, M; Van Sauers, A; Bond, N; Hawkins, W; Mans, D; Lichtveld, M

    2017-06-01

    Agricultural pesticides are widely used in Suriname, an upper middle-income Caribbean country located in South America. Suriname imported 1.8 million kg of agricultural pesticides in 2015. So far, however, national monitoring of pesticides in crops is absent. Reports from the Netherlands on imported Surinamese produce from 2010 to 2015 consistently showed that samples exceeded plant-specific pesticide maximum residue limits (MRLs) of the European Union (EU). Consumption of produce containing unsafe levels of pesticide residues can cause neurological disorders, and particularly, pregnant women and children may be vulnerable. This pilot study assessed the presence of pesticide residues in commonly consumed produce items cultivated in Suriname. Thirty-two insecticides (organophosphates, organochlorines, carbamates, and pyrethroids) and 12 fungicides were evaluated for their levels in nine types of produce. Pesticide residue levels exceeding MRLs in this study regarded cypermethrin (0.32 μg/g) in tomatoes (USA MRL 0.20 μg/g), lambda-cyhalothrin (1.08 μg/g) in Chinese cabbage (USA MRL 0.40 μg/g), endosulfan (0.07 μg/g) in tannia (EU MRL 0.05 μg/g), and lindane (0.02 and 0.03 μg/g, respectively) in tannia (EU MRL 0.01 μg/g). While only a few pesticide residues were detected in this small pilot study, these residues included two widely banned pesticides (endosulfan and lindane). There is a need to address environmental policy gaps. A more comprehensive sampling and analysis of produce from Suriname is warranted to better understand the scope of the problem. Preliminary assessments, using intake rate, hazard quotient, and level of concern showed that it is unlikely that daily consumption of tannia leads to adverse health effects.

  14. Presence of pesticide residues on produce cultivated in Suriname

    PubMed Central

    Wickliffe, J.; Wilson, M.; Van Sauers, A.; Bond, N.; Hawkins, W.; Mans, D.; Lichtveld, M.

    2017-01-01

    Agricultural pesticides are widely used in Suriname, an upper middle-income Caribbean country located in South America. Suriname imported 1.8 million kg of agricultural pesticides in 2015. So far, however, national monitoring of pesticides in crops is absent. Reports from the Netherlands on imported Surinamese produce from 2010 to 2015 consistently showed that samples exceeded plant-specific pesticide maximum residue limits (MRLs) of the European Union (EU). Consumption of produce containing unsafe levels of pesticide residues can cause neurological disorders, and particularly, pregnant women and children may be vulnerable. This pilot study assessed the presence of pesticide residues in commonly consumed produce items cultivated in Suriname. Thirty-two insecticides (organophosphates, organochlorines, carbamates, and pyrethroids) and 12 fungicides were evaluated for their levels in nine types of produce. Pesticide residue levels exceeding MRLs in this study regarded cypermethrin (0.32 μg/g) in tomatoes (USA MRL 0.20 μg/g), lambda-cyhalothrin (1.08 μg/g) in Chinese cabbage (USA MRL 0.40 μg/g), endosulfan (0.07 μg/g) in tannia (EU MRL 0.05 μg/g), and lindane (0.02 and 0.03 μg/g, respectively) in tannia (EU MRL 0.01 μg/g). While only a few pesticide residues were detected in this small pilot study, these residues included two widely banned pesticides (endosulfan and lindane). There is a need to address environmental policy gaps. A more comprehensive sampling and analysis of produce from Suriname is warranted to better understand the scope of the problem. Preliminary assessments, using intake rate, hazard quotient, and level of concern showed that it is unlikely that daily consumption of tannia leads to adverse health effects. PMID:28567597

  15. Direct gas-solid carbonation of serpentinite residues in the absence and presence of water vapor: a feasibility study for carbon dioxide sequestration.

    PubMed

    Veetil, Sanoopkumar Puthiya; Pasquier, Louis-César; Blais, Jean-François; Cecchi, Emmanuelle; Kentish, Sandra; Mercier, Guy

    2015-09-01

    Mineral carbonation of serpentinite mining residue offers an environmentally secure and permanent storage of carbon dioxide. The strategy of using readily available mining residue for the direct treatment of flue gas could improve the energy demand and economics of CO2 sequestration by avoiding the mineral extraction and separate CO2 capture steps. The present is a laboratory scale study to assess the possibility of CO2 fixation in serpentinite mining residues via direct gas-solid reaction. The degree of carbonation is measured both in the absence and presence of water vapor in a batch reactor. The gas used is a simulated gas mixture reproducing an average cement flue gas CO2 composition of 18 vol.% CO2. The reaction parameters considered are temperature, total gas pressure, time, and concentration of water vapor. In the absence of water vapor, the gas-solid carbonation of serpentinite mining residues is negligible, but the residues removed CO2 from the feed gas possibly due to reversible adsorption. The presence of small amount of water vapor enhances the gas-solid carbonation, but the measured rates are too low for practical application. The maximum CO2 fixation obtained is 0.07 g CO2 when reacting 1 g of residue at 200 °C and 25 barg (pCO2 ≈ 4.7) in a gas mixture containing 18 vol.% CO2 and 10 vol.% water vapor in 1 h. The fixation is likely surface limited and restricted due to poor gas-solid interaction. It was identified that both the relative humidity and carbon dioxide-water vapor ratio have a role in CO2 fixation regardless of the percentage of water vapor.

  16. Pesticides in persimmons, jujubes and soil from China: Residue levels, risk assessment and relationship between fruits and soils.

    PubMed

    Liu, Yihua; Li, Shiliang; Ni, Zhanglin; Qu, Minghua; Zhong, Donglian; Ye, Caifen; Tang, Fubin

    2016-01-15

    Extreme and uncontrolled usage of pesticides produces a number of problems for vegetation and human health. In this study, the existence of organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and fungicides (FUs) were investigated in persimmons/jujubes and their planted soils, which were collected from China. One OP (dimethoate), three OCs (DDT, quintozene and aldrin), six PYs (bifenthrin, fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin) and two FUs (triadimefon and buprofezin) were found in 36.4% of persimmons and 70.8% of jujubes, with concentrations from 1.0 μg/kg to 2945.0 μg/kg. The most frequently detected pesticides in the two fruits were fenpropathrin in persimmons and cypermethrin in jujubes, with the detection frequencies of 30.0% and 22.7%, respectively. The residues of 4.5% (persimmon) and 25.0% (jujube) of samples were higher than the maximum residue limits (MRLs) of China. Compared with the fruits, more types of pesticides and higher residues were observed in their planted soils. The most frequently detected pesticides were HCH in persimmon soil and DDT in jujube soil, with the detection frequencies of 10.9% and 12.7%, respectively. For the tested samples, 39.1% of fruit samples and 63.0% of soil samples with multiple residues (containing more than two pesticides) were noted, even up to 8 residues in fruits and 14 residues in soils. Except for cyhalothrin, the other short-term risks for the tested pesticides in the fruits were below 10%, and the highest long-term risk was 14.13% for aldrin and dieldrin. There was no significant health risk for consumers via consumption of the two fruits. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. High throughput-screening of animal urine samples: It is fast but is it also reliable?

    PubMed

    Kaufmann, Anton

    2016-05-01

    Advanced analytical technologies like ultra-high-performance liquid chromatography coupled to high resolution mass spectrometry can be used for veterinary drug screening of animal urine. The technique is sufficiently robust and reliable to detect veterinary drugs in urine samples of animals where the maximum residue limit of these compounds in organs like muscle, kidney, or liver has been exceeded. The limitations and possibilities of the technique are discussed. The most critical point is the variability of the drug concentration ratio between the tissue and urine. Ways to manage the false positive and false negatives are discussed. The capability to confirm findings and the possibility of semi-targeted analysis are also addressed. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  18. Recent developments in analysis of crack propagation and fracture of practical materials. [stress analysis in aircraft structures

    NASA Technical Reports Server (NTRS)

    Hardrath, H. F.; Newman, J. C., Jr.; Elber, W.; Poe, C. C., Jr.

    1978-01-01

    The limitations of linear elastic fracture mechanics in aircraft design and in the study of fatigue crack propagation in aircraft structures are discussed. NASA-Langley research to extend the capabilities of fracture mechanics to predict the maximum load that can be carried by a cracked part and to deal with aircraft design problems are reported. Achievements include: (1) improved stress intensity solutions for laboratory specimens; (2) fracture criterion for practical materials; (3) crack propagation predictions that account for mean stress and high maximum stress effects; (4) crack propagation predictions for variable amplitude loading; and (5) the prediction of crack growth and residual stress in built-up structural assemblies. These capabilities are incorporated into a first generation computerized analysis that allows for damage tolerance and tradeoffs with other disciplines to produce efficient designs that meet current airworthiness requirements.

  19. Effect of additives on the tensile performance and protein solubility of industrial oilseed residual based plastics.

    PubMed

    Newson, William R; Kuktaite, Ramune; Hedenqvist, Mikael S; Gällstedt, Mikael; Johansson, Eva

    2014-07-16

    Ten chemical additives were selected from the literature for their proposed modifying activity in protein-protein interactions. These consisted of acids, bases, reducing agents, and denaturants and were added to residual deoiled meals of Crambe abyssinica (crambe) and Brassica carinata (carinata) to modify the properties of plastics produced through hot compression molding at 130 °C. The films produced were examined for tensile properties, protein solubility, molecular weight distribution, and water absorption. Of the additives tested, NaOH had the greatest positive effect on tensile properties, with increases of 105% in maximum stress and 200% in strain at maximum stress for crambe and a 70% increase in strain at maximum stress for carinata. Stiffness was not increased by any of the applied additives. Changes in tensile strength and elongation for crambe and elongation for carinata were related to changes in protein solubility. Increased pH was the most successful in improving the protein aggregation and mechanical properties within the complex chemistry of residual oilseed meals.

  20. DECONV-TOOL: An IDL based deconvolution software package

    NASA Technical Reports Server (NTRS)

    Varosi, F.; Landsman, W. B.

    1992-01-01

    There are a variety of algorithms for deconvolution of blurred images, each having its own criteria or statistic to be optimized in order to estimate the original image data. Using the Interactive Data Language (IDL), we have implemented the Maximum Likelihood, Maximum Entropy, Maximum Residual Likelihood, and sigma-CLEAN algorithms in a unified environment called DeConv_Tool. Most of the algorithms have as their goal the optimization of statistics such as standard deviation and mean of residuals. Shannon entropy, log-likelihood, and chi-square of the residual auto-correlation are computed by DeConv_Tool for the purpose of determining the performance and convergence of any particular method and comparisons between methods. DeConv_Tool allows interactive monitoring of the statistics and the deconvolved image during computation. The final results, and optionally, the intermediate results, are stored in a structure convenient for comparison between methods and review of the deconvolution computation. The routines comprising DeConv_Tool are available via anonymous FTP through the IDL Astronomy User's Library.

  1. A comparison of measures of riverbed form for evaluating distributions of benthic fishes

    USGS Publications Warehouse

    Wildhaber, Mark L.; Lamberson, Peter J.; Galat, David L.

    2003-01-01

    A method to quantitatively characterize the bed forms of a large river and a preliminary test of the relationship between bed-form characteristics and catch per unit area of benthic fishes is presented. We used analog paper recordings of bathymetric data from the Missouri River and fish data collected from 1996 to 1998 at both the segment (???101-102-km) and macrohabitat (???10-1-100-km) spatial scales. Bed-form traces were transformed to digital data with image analysis software. The slope, mean residual, and SD of the residuals of the regression of depth versus distance along the bottom, as well as mean depth, were estimated for each trace. These four metrics were compared with sinuosity, fractal dimension, critical scale, and maximum mean angle for the same traces. Mean depth and sinuosity differed among segments and macrohabitats. Fractal-based measures of the relative depth of bottom troughs (critical scale) and smoothness (maximum mean angle) differed among segments. Statistics-based measures of the relative depth of bottom troughs (mean residual) and smoothness (SD of the residuals) differed among macrohabitats. Sites with shovelnose sturgeon Scaphirhynchus platorynchus were shallower and smoother than sites without shovelnose sturgeon. When compared with sites without sicklefin chub Macrhybopsis meeki, sites with sicklefin chub were shallower, had shallower troughs, and sloped more out of the flow of the river. Sites with sturgeon chub M. gelida were shallower, had shallower troughs, and were smoother than sites without sturgeon chub. Sites with and without channel catfish Ictalurus punctatus did not differ for any bed-form variables measured. Nonzero shovelnose sturgeon density increased with depth, whereas nonzero sturgeon chub density decreased with depth. Indices of bed-form structure demonstrated potential for describing the distribution and abundance of Missouri River benthic fishes. The observed fish patterns, though limited, provide valuable direction for future research into the habitat preferences of these fishes.

  2. High-throughput enzyme screening platform for the IPP-bypass mevalonate pathway for isopentenol production

    DOE PAGES

    Kang, Aram; Meadows, Corey W.; Canu, Nicolas; ...

    2017-04-05

    Isopentenol (or isoprenol, 3-methyl-3-buten-1-ol) is a drop-in biofuel and a precursor for commodity chemicals such as isoprene. Biological production of isopentenol via the mevalonate pathway has been optimized extensively in Escherichia coli, yielding 70% of its theoretical maximum. However, high ATP requirements and isopentenyl diphosphate (IPP) toxicity pose immediate challenges for engineering bacterial strains to overproduce commodities utilizing IPP as an intermediate. To overcome these limitations, we developed an “IPP-bypass” isopentenol pathway using the promiscuous activity of a mevalonate diphosphate decarboxylase (PMD) and demonstrated improved performance under aeration-limited conditions. However, relatively low activity of PMD toward the non-native substrate (mevalonatemore » monophosphate, MVAP) was shown to limit flux through this new pathway. By inhibiting all IPP production from the endogenous non-mevalonate pathway, we developed a high-throughput screening platform that correlated promiscuous PMD activity toward MVAP with cellular growth. Successful identification of mutants that altered PMD activity demonstrated the sensitivity and specificity of the screening platform. Strains with evolved PMD mutants and the novel IPP-bypass pathway increased titers up to 2.4-fold. Further enzymatic characterization of the evolved PMD variants suggested that higher isopentenol titers could be achieved either by altering residues directly interacting with substrate and cofactor or by altering residues on nearby α-helices. These altered residues could facilitate the production of isopentenol by tuning either k cat or K i of PMD for the non-native substrate. The synergistic modification made on PMD for the IPP-bypass mevalonate pathway is expected to significantly facilitate the industrial scale production of isopentenol.« less

  3. High-throughput enzyme screening platform for the IPP-bypass mevalonate pathway for isopentenol production

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kang, Aram; Meadows, Corey W.; Canu, Nicolas

    Isopentenol (or isoprenol, 3-methyl-3-buten-1-ol) is a drop-in biofuel and a precursor for commodity chemicals such as isoprene. Biological production of isopentenol via the mevalonate pathway has been optimized extensively in Escherichia coli, yielding 70% of its theoretical maximum. However, high ATP requirements and isopentenyl diphosphate (IPP) toxicity pose immediate challenges for engineering bacterial strains to overproduce commodities utilizing IPP as an intermediate. To overcome these limitations, we developed an “IPP-bypass” isopentenol pathway using the promiscuous activity of a mevalonate diphosphate decarboxylase (PMD) and demonstrated improved performance under aeration-limited conditions. However, relatively low activity of PMD toward the non-native substrate (mevalonatemore » monophosphate, MVAP) was shown to limit flux through this new pathway. By inhibiting all IPP production from the endogenous non-mevalonate pathway, we developed a high-throughput screening platform that correlated promiscuous PMD activity toward MVAP with cellular growth. Successful identification of mutants that altered PMD activity demonstrated the sensitivity and specificity of the screening platform. Strains with evolved PMD mutants and the novel IPP-bypass pathway increased titers up to 2.4-fold. Further enzymatic characterization of the evolved PMD variants suggested that higher isopentenol titers could be achieved either by altering residues directly interacting with substrate and cofactor or by altering residues on nearby α-helices. These altered residues could facilitate the production of isopentenol by tuning either k cat or K i of PMD for the non-native substrate. The synergistic modification made on PMD for the IPP-bypass mevalonate pathway is expected to significantly facilitate the industrial scale production of isopentenol.« less

  4. Residue analysis of four diacylhydrazine insecticides in fruits and vegetables by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method using ultra-performance liquid chromatography coupled to tandem mass spectrometry.

    PubMed

    Liu, Xingang; Xu, Jun; Dong, Fengshou; Li, Yuanbo; Song, Wenchen; Zheng, Yongquan

    2011-08-01

    The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds was achieved in less than 3.0 min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide, and halofenozide and in negative mode (ESI-) for chromafenozide. The limits of detection were below 0.6 μg kg(-1), while the limit of quantification did not exceed 2 μg kg(-1) in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and 1 mg kg(-1)). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged from 74.2% to 112.5% with RSDs in the range of 1.4-13.8% (n = 5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical method for diacylhydrazine insecticide in vegetables and fruits.

  5. Endoscopic endonasal surgery for giant pituitary adenomas: advantages and limitations.

    PubMed

    Koutourousiou, Maria; Gardner, Paul A; Fernandez-Miranda, Juan C; Paluzzi, Alessandro; Wang, Eric W; Snyderman, Carl H

    2013-03-01

    Giant pituitary adenomas (> 4 cm in maximum diameter) represent a significant surgical challenge. Endoscopic endonasal surgery (EES) has recently been introduced as a treatment option for these tumors. The authors present the results of EES for giant adenomas and analyze the advantages and limitations of this technique. The authors retrospectively reviewed the medical files and imaging studies of 54 patients with giant pituitary adenomas who underwent EES and studied the factors affecting surgical outcome. Preoperative visual impairment was present in 45 patients (83%) and partial or complete pituitary deficiency in 28 cases (52%), and 7 patients (13%) presented with apoplexy. Near-total resection (> 90%) was achieved in 36 patients (66.7%). Vision was improved or normalized in 36 cases (80%) and worsened in 2 cases due to apoplexy of residual tumor. Significant factors that limited the degree of resection were a multilobular configuration of the adenoma (p = 0.002) and extension to the middle fossa (p = 0.045). Cavernous sinus invasion, tumor size, and intraventricular or posterior fossa extension did not influence the surgical outcome. Complications included apoplexy of residual adenoma (3.7%), permanent diabetes insipidus (9.6%), new pituitary insufficiency (16.7%), and CSF leak (16.7%, which was reduced to 7.4% in recent years). Fourteen patients underwent radiation therapy after EES for residual mass or, in a later stage, for recurrence, and 10 with functional pituitary adenomas received medical treatment. During a mean follow-up of 37.9 months (range 1-114 months), 7 patients were reoperated on for tumor recurrence. Three patients were lost to follow-up. Endoscopic endonasal surgery provides effective initial management of giant pituitary adenomas with favorable results compared with traditional microscopic transsphenoidal and transcranial approaches.

  6. Usage, residue, and human health risk of antibiotics in Chinese aquaculture: A review.

    PubMed

    Liu, Xiao; Steele, Joshua Caleb; Meng, Xiang-Zhou

    2017-04-01

    Aquaculture is a booming industry in the world and China is the largest producer and exporter of aquatic products. To prevent and treat diseases occurred in aquaculture, antibiotics are widely applied. However, the information of antibiotics used in Chinese aquaculture is still limited. Based on peer-reviewed papers, documents, reports, and even farmer surveys, this review summarized antibiotics used in Chinese aquaculture. In 2014, more than 47.4 million tonnes of farmed aquatic products were produced in mainland China. The outputs in the east and south parts of China can reach as much as 600 times higher than those in the northwest areas, which is clearly separated by the "Hu Line" - a line that marks a striking difference in the distribution of population. A total of 20 antibiotics belonging to eight categories have been reported for use, mainly via oral administration. However, only 13 antibiotics have been authorized for application in Chinese aquaculture and 12 antibiotics used are not authorized. Totally, 234 cases on antibiotic residues in Chinese aquatic products were recorded, including 24 fish species, eight crustacean species, and four mollusk species. Thirty-two antibiotics have been detected in aquatic products; quinolones and sulfonamides were the dominated residual chemicals. For specific compound, ciprofloxacin, norfloxacin, and sulfisoxazole have the highest concentrations. Except for a few cases, all residual concentrations were lower than the maximum residue limits. Through the consumption of aquatic products tainted by antibiotics, humans may acquire adverse drug reactions or antibiotic-resistant bacteria. However, the risk of antimicrobial resistance in human body, when exposed to antibiotics at sub-inhibitory concentrations, has not been exhaustively considered in the risk assessment. In addition, a national comprehensive investigation on the amount of antibiotics used in Chinese aquaculture is still needed in future studies. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Comparing water, bovine milk, and indoor residual spraying as possible sources of DDT and pyrethroid residues in breast milk.

    PubMed

    Sereda, Barbara; Bouwman, Henk; Kylin, Henrik

    2009-01-01

    The presence of pollutants in human breast milk is of major concern, especially in malaria control areas where 1,1,1-trichloro-2,2-bis(4-chlorophenyl) ethane (DDT) is currently used as indoor residual spray (IRS). The levels of DDT and pyrethroids (PYR) were determined in breast milk, bovine milk, and drinking water from northern KwaZulu-Natal, South Africa. Both reference and exposed mothers used the same market food, but the DDT levels in the exposed mothers (mean SigmaDDT 10 microg/g milk fat [mf]) were much higher than for the reference mothers (mean SigmaDDT 1.3 microg/g milk fat). This difference in residue levels indicates uptake from IRS-applied DDT, most likely via air and skin contact, and excludes food as the main source of pollutants. DDT levels in bovine milk (mean SigmaDDT 0.15 microg/g mf) from the exposed area were less than levels in breast milk from the reference area, and lower than the 20 microg/L maximum residue limit (MRL) set by the Food and Agriculture Organization (FAO). Mean SigmaDDT in water was 0.0065 microg/L, much lower then the WHO limit of the sum of all metabolites in drinking water of 1 microg/L, and therefore highly unlikely to have contributed to any extent toward levels in breast milk. Permethrin in breast milk (mean 1.1-1.6 microg/g milk fat) was probably derived from home garden and indoor use, while the other PYR (cypermethrin and cyfluthrin) at lower concentrations were probably derived from food and agricultural exposure. It is postulated that a better understanding of the indoor dynamics of DDT and other insecticides, through a concept of Total Homestead Environment Approach (THEA), is crucial for investigating options of reducing human exposure and uptake under malaria control conditions.

  8. Determination of 17 Organophosphate Pesticide Residues in Mango by Modified QuEChERS Extraction Method Using GC-NPD/GC-MS and Hazard Index Estimation in Lucknow, India

    PubMed Central

    Srivastava, Ashutosh K.; Rai, Satyajeet; Srivastava, M. K.; Lohani, M.; Mudiam, M. K. R.; Srivastava, L. P.

    2014-01-01

    A total of 162 samples of different varieties of mango: Deshehari, Langra, Safeda in three growing stages (Pre-mature, Unripe and Ripe) were collected from Lucknow, India, and analyzed for the presence of seventeen organophosphate pesticide residues. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method of extraction coupled with gas chromatography was validated for pesticides and qualitatively confirmed by gas chromatography- mass spectrometry. The method was validated with different concentrations of mixture of seventeen organophosphate pesticides (0.05, 0.10, 0.50 mg kg−1) in mango. The average recovery varied from 70.20% to 95.25% with less than 10% relative standard deviation. The limit of quantification of different pesticides ranged from 0.007 to 0.033 mg kg−1. Out of seventeen organophosphate pesticides only malathion and chlorpyriphos were detected. Approximately 20% of the mango samples have shown the presence of these two pesticides. The malathion residues ranged from ND-1.407 mg kg−1 and chlorpyriphos ND-0.313 mg kg−1 which is well below the maximum residues limit (PFA-1954). In three varieties of mango at different stages from unpeeled to peeled sample reduction of malathion and chlorpyriphos ranged from 35.48%–100% and 46.66%–100% respectively. The estimated daily intake of malathion ranged from 0.032 to 0.121 µg kg−1 and chlorpyriphos ranged from zero to 0.022 µg kg−1 body weight from three different stages of mango. The hazard indices ranged from 0.0015 to 0.0060 for malathion and zero to 0.0022 for chlorpyriphos. It is therefore indicated that seasonal consumption of these three varieties of mango may not pose any health hazards for the population of Lucknow, city, India because the hazard indices for malathion and chlorpyriphos residues were below to one. PMID:24809911

  9. Determination of six pyrethroid insecticides in fruit juice samples using dispersive liquid-liquid microextraction combined with high performance liquid chromatography.

    PubMed

    Boonchiangma, Suthasinee; Ngeontae, Wittaya; Srijaranai, Supalax

    2012-01-15

    Dispersive liquid-liquid microextraction (DLLME) coupled to high performance liquid chromatography (HPLC) with UV detection was applied for the determination of six pyrethroids (tetramethrin, fenpropathrin, cypermethrin, deltamethrin, fenvalerate and permethrin) in various fruit juices including apple, red grape, orange, kiwi, passion fruit, pomegranate and guava juice. Six pyrethroids were separated within 30 min using a Waters Atlantis T3 column under an isocratic elution of acetonitrile-water (72:28). The parameters affecting extraction efficiency of the DLLME method such as type of disperser and extraction solvent, volume of disperser and extraction solvent and centrifugation time were investigated. Under the optimum conditions, 5.00 mL of sample solution, 300 μL of chloroform as extraction solvent and 1.25 mL of methanol as dispersive solvent gave high enrichment factor in the range of 62-84. Good linearity was obtained from 2 to 1,500 μg/L (r(2)>0.995). The mean recoveries of the pyrethroids evaluated by fortification of real samples were in the range of 84-94%. The limits of detection ranging from 2 to 5 μg/L are sufficient to analyze pyrethroid residues at the maximum residue limits (MRLs) established by the European Union (EU) in fruit juices. The proposed method can be applied to direct determination of pyrethroid residues in fruit juices. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Quantitative Multiclass Pesticide Residue Analysis in Apple, Pear, and Grape by Modified QuEChERS and Liquid Chromatography Coupled to High-Resolution Mass Spectrometry.

    PubMed

    Munaretto, Juliana S; Viera, Mariela de S; Martins, Manoel L; Adaime, Martha B; Zanella, Renato

    2016-11-01

    Most of the analytical methods currently applied in food control laboratories are focused on the determination of target compounds using LC coupled to tandem MS, which is an effective technique, but low-resolution MS is limited. Thus, a method for determination of pesticide multiresidues in fruits (pear, apple, and grape) using a modified quick, easy, cheap, effective, rugged, and safe method and LC coupled to quadrupole time-of-flight (Q-TOF) MS was developed and validated. The proposed method showed good linearity (r2 > 0.99) from 1 to 100 μg/L. Recoveries for blank samples spiked at 0.01, 0.04, and 0.10 mg/kg were between 66 and 122%, with RSDs <28%. Respective LOQs for apple, pear, and grape matrixes were 0.01 mg/kg for 112, 120, and 118 compounds, and 0.04 mg/kg for 22, 12, and 17 compounds, and average mass accuracy error was 3.2 ppm. LC with Q-TOF MS detection using protonated molecular ion and/or adducts and mass accuracy provided reliability for the method. The proposed method is effective for pesticide residue determination in apple, pear, and grape samples, proving that high-resolution MS using full scan mode can be a powerful and reliable technique for quantification purposes, being adequate for application in the surveillance of maximum residue limits set by different legislations.

  11. Development and validation of a solid-phase extraction method coupled to liquid chromatography with fluorescence detection for the determination of fluoroquinolone residues in powdered infant formulae. Application to the analysis of samples from the Spanish and Latin American market.

    PubMed

    Rodriguez, E; Moreno-Bondi, M C; Marazuela, M D

    2008-10-31

    This paper describes a new method for the effective extraction, clean-up and chromatographic analysis of residues of four fluoroquinolones (ciprofloxacin, enrofloxacin, danofloxacin and sarafloxacin) in powdered infant formulae and follow-on preparations. Samples were reconstituted following the manufacturer's recommendations and treated with trichloroacetic acid in methanol 10% (w/v) for deproteinization. Two solid-phase extraction cartridges have been evaluated for sample clean-up and preconcentration, Strata Screen A and Strata X and the later provided the best recoveries for all the analytes tested. Chromatographic analysis has been carried out using a polar endcapped column (AQUA C(18)) and fluorescence detection, with lomefloxacin (LOME) as internal standard. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(alpha)) and detection capability (CC(beta)). Typical recoveries ranged between 70 and 110% at levels below and above the maximum residue limits of the target analytes in bovine milk, with an excellent intralab reproducibility (RSDs<7%). Matrix effects did not significantly affect method accuracy, as evidenced by analyzing different brands of milk. The method has been successfully applied to the analysis of 100 samples of infant and follow-on formulae of the Spanish and Latin American market, using LC-MS/MS as confirmatory technique.

  12. Determination of metoserpate, buquinolate, and diclofenac in pork, eggs, and milk using liquid chromatography-tandem mass spectrometry.

    PubMed

    Park, Jin-A; Abd El-Aty, A M; Zheng, Weijia; Kim, Seong-Kwan; Choi, Jeong-Min; Hacımüftüoğlu, Ahmet; Shim, Jae-Han; Shin, Ho-Chul

    2018-06-01

    In this work, a method was developed for the simultaneous determination of residual metoserpate, buquinolate and diclofenac in pork, milk, and eggs. Samples were extracted with 0.1% formic acid in acetonitrile, defatted with n-hexane, and filtered prior to analysis using liquid chromatography-tandem mass spectrometry. The analytes were separated on a C 18 column using 0.1% acetic acid and methanol as the mobile phase. The matrix-matched calibration curves showed good linearity over a concentration range of 5-50 ng/g with coefficients of determination (R 2 ) ≥0.991. The intra- and inter-day accuracies (expressed as recovery percentage values) calculated using three spiking levels (5, 10, and 20 μg/kg) were 80-108.65 and 74.06-107.15%, respectively, and the precisions (expressed as relative standard deviation) were 2.86-13.67 and 0.05-11.74%, respectively, for the tested drugs determined in various matrices. The limits of quantification (1 and 2 μg/kg) were below the uniform residual level (0.01 mg/kg) set for compounds that have no specific maximum residue limit (MRL). The developed method was tested using market samples and none of the target analytes was detected in any of the samples. The validated method proved to be practicable for detection of the tested analytes in pork, milk, and eggs. Copyright © 2018 John Wiley & Sons, Ltd.

  13. Dissipation kinetics of emamectin benzoate and lufenuron residues in cabbage grown under field conditions.

    PubMed

    Dong, Bizhang; Zhao, Qing; Hu, Jiye

    2015-12-01

    Residue analysis of emamectin benzoate and lufenuron in cabbage matrices and soil was developed using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and ultra high-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile (v/v) or 1% acetic acid in acetonitrile/water (5:1, v/v) and cleaned up by dispersive solid-phase extraction. Mean recoveries and relative standard deviations (RSDs) in all samples ranged 87.8-100.0 % and 3.6-12.6% for emamectin benzoate and 87.8-104.8 % and 6.2-11.5% for lufenuron, respectively. The validated method was used to evaluate the dissipation rate of emamectin benzoate and lufenuron in cabbage and soil as well as the residual levels in harvested cabbage and soil at different preharvest intervals (PHI). The half-lives of emamectin benzoate and lufenuron were 1.08-2.70 and 1.74-5.04 days in cabbage, and 1.42-4.01 and 0.94-6.18 days in soil, respectively. The terminal residues were below the China maximum residue limits (MRLs) at 3 days for emamectin benzoate (0.1 mg kg(-1)) and European Union MRLs at 5 days for lufenuron (0.5 mg kg(-1)), which suggested that 5 days could be recommended as the PHI for the commercial formulation of emamectin benzoate and lufenuron application in the Chinese cabbage field.

  14. Multi-residue analysis of pesticide residues in mangoes using solid-phase microextraction coupled to liquid chromatography and UV-Vis detection.

    PubMed

    Filho, Adalberto M; dos Santos, Fábio N; Pereira, Pedro A de Paula

    2011-11-01

    A sensitive and efficient solid-phase microextraction method, based on liquid chromatography and UV-Vis detection, was developed and validated as an alternative method for sample screening prior to LC-MS analysis. It enables the simultaneous determination of ten pesticides in mango fruits. The fiber used was polydimethylsiloxane while optimum SPME conditions employed have been developed and optimized in a previous work. The desorption process was performed in static mode, using acetonitrile as a solvent. The results indicate that the DI-SPME/HPLC/UV-Vis procedure resulted in good linear range, accuracy, precision and sensibility and is adequate for analyzing pesticide residues in mango fruits. The limits of detection (0.6-3.3 μg/kg) and quantification (2.0-10.0 μg/kg) were achieved with values lower than the maximum residue levels (MRLs) established by Brazilian legislation for all pesticides in this study. The average recovery rates obtained for each pesticide ranged from 71.6 to 104.3% at three fortification levels, with the relative standard deviation ranging from 4.3 to 18.6%. The proposed method was applied for the determination of the aforementioned compounds in commercial mango samples and residues of azoxystrobin, fenthion, permethrin, abamectin and bifenthrin were detected in the mango samples, although below the MRLs established by Brazilian legislation. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Dissipation behaviour, residue distribution and dietary risk assessment of tetraconazole and kresoxim-methyl in greenhouse strawberry via RRLC-QqQ-MS/MS technique.

    PubMed

    Chen, Xiaoxin; Fan, Xueqi; Ma, Yecheng; Hu, Jiye

    2018-02-01

    20% commercial suspension emulsion (SE) of (8% tetraconazole + 12% kresoxim-methyl), as a pre-registered product in China, was firstly investigated under Chinese greenhouse-field conditions. A MWCNTs-based QuEChERS method for simultaneous determination of tetraconazole and kresoxim-methyl in strawberry was developed and validated via RRLC-QqQ-MS/MS. On basis of this method, the dissipation behaviours, residue distributions and dietary risk probability of these fungicides in strawberry were further investigated for food safety. The dissipations of tetraconazole and kresoxim-methyl followed first-order kinetics with the half-lives of 8.0-18.2 days. The highest residues (HRs) of these fungicides in the supervised trials at the pre-harvest interval (PHI, 3 days) were below 0.8970mgkg -1 . The total national estimated daily intake (NEDI) of tetraconazole and kresoxim-methy in strawberry at the PHI 3day was 0.2784mg and 0.4031mg, respectively, based on Chinese dietary pattern and terminal residue distributions under good agricultural practices (GAP) conditions. The risk quotients (RQs) of tetraconazole and kresoxim-methy at PHI 3 days were below 82.7% and 1.6%, respectively, showing that the evaluated strawberry exhibited an acceptably low dietary risk to consumers. The current study could not only guide reasonable usage of the formulation, but also facilitate the setting of maximum residue limits (MRLs) of tetraconazole in strawberry. Copyright © 2017 Elsevier Inc. All rights reserved.

  16. AFNOR validation of Premi Test, a microbiological-based screening tube-test for the detection of antimicrobial residues in animal muscle tissue.

    PubMed

    Gaudin, Valerie; Juhel-Gaugain, Murielle; Morétain, Jean-Pierre; Sanders, Pascal

    2008-12-01

    Premi Test contains viable spores of a strain of Bacillus stearothermophilus which is sensitive to antimicrobial residues, such as beta-lactams, tetracyclines, macrolides and sulphonamides. The growth of the strain is inhibited by the presence of antimicrobial residues in muscle tissue samples. Premi Test was validated according to AFNOR rules (French Association for Normalisation). The AFNOR validation was based on the comparison of reference methods (French Official method, i.e. four plate test (FPT) and the STAR protocol (five plate test)) with the alternative method (Premi Test). A preliminary study was conducted in an expert laboratory (Community Reference Laboratory, CRL) on both spiked and incurred samples (field samples). Several method performance criteria (sensitivity, specificity, relative accuracy) were estimated and are discussed, in addition to detection capabilities. Adequate agreement was found between the alternative method and the reference methods. However, Premi Test was more sensitive to beta-lactams and sulphonamides than the FPT. Subsequently, a collaborative study with 11 laboratories was organised by the CRL. Blank and spiked meat juice samples were sent to participants. The expert laboratory (CRL) statistically analysed the results. It was concluded that Premi Test could be used for the routine determination of antimicrobial residues in muscle of different animal origin with acceptable analytical performance. The detection capabilities of Premi Test for beta-lactams (amoxicillin, ceftiofur), one macrolide (tylosin) and tetracycline were at the level of the respective maximum residue limits (MRL) in muscle samples or even lower.

  17. Methylene Blue Removal by Biochars from Food Industry By-Products

    NASA Astrophysics Data System (ADS)

    Orfanos, Alexis; Manariotis, Ioannis D.; Karapanagioti, Hrissi K.

    2016-04-01

    Biomass produced by food industries is mainly used as feedstock or in composting. In recent years, considerable research effort has been focused on the production of biochar under oxygen-limited conditions from carbon-rich biomass, such as food industry by-products, as mitigation measure for global warming once it is used as a soil amendment. The present study presents the findings of an experimental work, which investigated the use of different biochars for the removal of methylene blue (MB) from aqueous solutions. Biochars were produced from malt spent rootlets (MSR) from brewering and espresso coffee residue from coffee shops. MSR was pyrolyzed at temperatures of 300, 400, 500, 750, 850, and 900oC and the coffee residue was pyrolyzed at 850oC. The charring process was performed under limited-oxygen conditions using specialized containers. The surface area and the porosity of the materials were determined. Batch experiments were conducted in order to evaluate the sorption capacity of the above materials, and samples were agitated for 24 h at 25oC, at an optimum pH of about 7. Kinetic analysis was conducted over a period of 24 h, and isotherm studies were also constructed. The surface area of biochar produced from MSR and the MB removal were considerably increased at pyrolysis temperatures higher than 500oC. At 850oC, the maximum surface area value (300 m2 g-1) was observed, and the MB sorption capacity was 99 mg g-1. Based on the kinetic experimental data, sorption capacities at 120 min were over 58% of their equilibrium values for the biochars used. The maximum MB sorption capacity, based on the isotherm data, was 130 mg g-1, for the two biochars employed.

  18. Thermal Residual Stress in Environmental Barrier Coated Silicon Nitride - Modeled

    NASA Technical Reports Server (NTRS)

    Ali, Abdul-Aziz; Bhatt, Ramakrishna T.

    2009-01-01

    When exposed to combustion environments containing moisture both un-reinforced and fiber reinforced silicon based ceramic materials tend to undergo surface recession. To avoid surface recession environmental barrier coating systems are required. However, due to differences in the elastic and thermal properties of the substrate and the environmental barrier coating, thermal residual stresses can be generated in the coated substrate. Depending on their magnitude and nature thermal residual stresses can have significant influence on the strength and fracture behavior of coated substrates. To determine the maximum residual stresses developed during deposition of the coatings, a finite element model (FEM) was developed. Using this model, the thermal residual stresses were predicted in silicon nitride substrates coated with three environmental coating systems namely barium strontium aluminum silicate (BSAS), rare earth mono silicate (REMS) and earth mono di-silicate (REDS). A parametric study was also conducted to determine the influence of coating layer thickness and material parameters on thermal residual stress. Results indicate that z-direction stresses in all three systems are small and negligible, but maximum in-plane stresses can be significant depending on the composition of the constituent layer and the distance from the substrate. The BSAS and REDS systems show much lower thermal residual stresses than REMS system. Parametric analysis indicates that in each system, the thermal residual stresses can be decreased with decreasing the modulus and thickness of the coating.

  19. Approach for Pesticide Residue Analysis for Metabolite Prothioconazole-desthio in Animal Origin Food.

    PubMed

    Liu, Hui; Yao, Guojun; Liu, Xueke; Liu, Chang; Zhan, Jing; Liu, Donghui; Wang, Peng; Zhou, Zhiqiang

    2017-03-22

    Food safety problems such as damage to immune, nervous, and endocrine systems leading to cancer and malformations have received increasing attention. To achieve the maximum residue limits, the most discussed method of high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) is widely used with a advantage of high precision and resolution. Prothioconazole is a broad-spectrum thiocarbamate fungicide. It can rapidly metabolize to prothioconazole-desthio in different matrixes. Rapid and effective methods for the determination of prothioconazole-desthio in five kinds of different animal food were developed. Samples were extracted with acetonitrile or acetonitrile/water and determined by HPLC-MS/MS. The limit of detection and limit of quantification values of prothioconazole-desthio were 0.015 and 0.05 mg/kg for porcine liver and kidney, 0.0015 and 0.005 mg/kg for pork, and 0.003 and 0.01 mg/kg for eggs, together with 0.0012 and 0.004 mg/kg for milk of the detected method, respectively. A good linear regression trend can be observed in a certain concentration range for all of the animal food. At fortified levels, recoveries were between 83.6 and 105%, with relative standard deviations of 1.5-10.3%. A sample survey of 150 samples with 30 samples for each kind of animal food across the country was conducted and found that there was no prothioconazole-desthio detected in all samples.

  20. Effects of leachate on geotechnical characteristics of sandy clay soil

    NASA Astrophysics Data System (ADS)

    Harun, N. S.; Ali, Z. Rahman; Rahim, A. S.; Lihan, T.; Idris, R. M. W.

    2013-11-01

    Leachate is a hazardous liquid that poses negative impacts if leaks out into environments such as soil and ground water systems. The impact of leachate on the downgraded quality in terms of chemical characteristic is more concern rather than the physical or mechanical aspect. The effect of leachate on mechanical behaviour of contaminated soil is not well established and should be investigated. This paper presents the preliminary results of the effects of leachate on the Atterberg limit, compaction and shear strength of leachate-contaminated soil. The contaminated soil samples were prepared by mixing the leachate at ratiosbetween 0% and 20% leachate contents with soil samples. Base soil used was residual soil originated from granitic rock and classified as sandy clay soil (CS). Its specific gravity ranged between 2.5 and 2.64 with clay minerals of kaolinite, muscovite and quartz. The field strength of the studied soil ranged between 156 and 207 kN/m2. The effects of leachate on the Atterberg limit clearly indicated by the decrease in liquid and plastic limit values with the increase in the leachate content. Compaction tests on leachate-contaminated soil caused the dropped in maximum dry density, ρdry and increased in optimum moisture content, wopt when the amount of leachate was increased between 0% and 20%. The results suggested that leachate contamination capable to modify some geotechnical properties of the studied residual soils.

  1. Evaluation of a new modified QuEChERS method for the monitoring of carbamate residues in high-fat cheeses by using UHPLC-MS/MS.

    PubMed

    Hamed, Ahmed M; Moreno-González, David; Gámiz-Gracia, Laura; García-Campaña, Ana M

    2017-01-01

    A simple and efficient method for the determination of 28 carbamates in high-fat cheeses is proposed. The methodology is based on a modified quick, easy, cheap, effective, rugged, and safe procedure as sample treatment using a new sorbent (Z-Sep + ) followed by ultra-high performance liquid chromatography with tandem mass spectrometry determination. The method has been validated in different kinds of cheese (Gorgonzola, Roquefort, and Camembert), achieving recoveries of 70-115%, relative standard deviations lower than 13% and limits of quantification lower than 5.4 μg/kg, below the maximum residue levels tolerated for these compounds by the European legislation. The matrix effect was lower than ±30% for all the studied pesticides. The combination of ultra-high performance liquid chromatography and tandem mass spectrometry with this modified quick, easy, cheap, effective, rugged, and safe procedure using Z-Sep + allowed a high sample throughput and an efficient cleaning of extracts for the control of these residues in cheeses with a high fat content. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Evaluation of the QuEChERS sample preparation approach for the analysis of pesticide residues in olives.

    PubMed

    Cunha, Sara C; Lehotay, Steven J; Mastovska, Katerina; Fernandes, José O; Beatriz, Maria; Oliveira, P P

    2007-03-01

    This paper describes the use of a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for extraction and cleanup of 16 pesticide residues of interest in olives and olive oil. These products contain a high lipid content, which can adversely affect pesticide recoveries and harm traditional chromatographic systems. For extraction, the main factors (oil and water content) were studied and optimized in experiments to maximize pesticide recoveries. Dispersive SPE with different sorbents was also investigated to minimize matrix coextractives and interferences. For analysis, a new automated DSI device was tested in GC-MS to avoid nonvolatile coextractives from contaminating the instrument. LC-MS/MS with positive ESI was used for those pesticides that were difficult to detect by GC-MS. The final method was validated for olives in terms of recoveries, repeatabilities, and reproducibilities using both detection techniques. The results demonstrated that the method achieved acceptable quantitative recoveries of 70-109% with RSDs < 20% for DSI-GC-MS and 88-130% with RSDs < 10% for LC-MS/MS, and LOQ at or below the regulatory maximum residue limits for the pesticides were achieved.

  3. Transfer rates of 19 typical pesticides and the relationship with their physicochemical property.

    PubMed

    Chen, Hongping; Pan, Meiling; Pan, Rong; Zhang, Minglu; Liu, Xin; Lu, Chengyin

    2015-01-21

    Determining the transfer rate of pesticides during tea brewing is important to identify the potential exposure risks from pesticide residues in tea. In this study, the transfer rates of 19 typical pesticides from tea to brewing were investigated using gas chromatography tandem mass and ultraperformance liquid chromatography tandem mass. The leaching rates of five pesticides (isocarbophos, triazophos, fenvalerate, buprofezin, and pyridaben) during tea brewing were first reported. The pesticides exhibited different transfer rates; however, this result was not related to residual concentrations and tea types. Pesticides with low octanol-water partition coefficients (Logkow) and high water solubility demonstrated high transfer rates. The transfer rates of pesticides with water solubility > 29 mg L(-1) (or <15 mg L(-1)) were >25% (or <10%), and those of pesticides with LogKow < 1.52 (or >2.48) were >65% (or <35%). This result indicates that water solubility at approximately 20 mg L(-1) and LogKow at approximately 2.0 could be the demarcation lines of transfer rate. The results of this study can be used as a guide in the application of pesticides to tea trees and establishment of maximum residue limits of pesticides in tea to reduce pesticide exposure in humans.

  4. Development of an enzyme-linked immunosorbent assay (ELISA) for residue analysis of the fungicide azoxystrobin in agricultural products.

    PubMed

    Kondo, Mika; Tsuzuki, Kazuyuki; Hamada, Hiroshi; Yamaguchi Murakami, Yukie; Uchigashima, Mikiko; Saka, Machiko; Watanabe, Eiki; Iwasa, Seiji; Narita, Hiroshi; Miyake, Shiro

    2012-02-01

    A direct competitive enzyme-linked immunosorbent assay (dc-ELISA) was developed for residue analysis of azoxystrobin in garden crops, for which the maximum residue limits (MRLs) are 0.5-50 mg/kg in Japan. For hapten synthesis, an ethyl carboxyl group was introduced to the 4-position of the 2-cyanophenoxy group in azoxystrobin, and its cyano group was changed to a methyl group. An anti-azoxystrobin monoclonal antibody was prepared from mice immunized with hapten-keyhole limpet hemocyanin conjugate. The dc-ELISA using prepared antibody showed 50-250-fold higher sensitivity compared to the MRLs. The working range of the dc-ELISA was 10-200 ng/mL. The dc-ELISA showed high specificity to azoxystrobin. When methanol extracts from nine kinds of garden crops spiked with azoxystrobin ranging near the MRLs were analyzed, the determined results by the dc-ELISA agreed well with the results of their controls. In addition, azoxystrobin spiked in garden crops homogenates was satisfactorily extracted by methanol solution and easily analyzed. The recovery rate of dc-ELISA was 96-109% and correlated well with the results obtained by HPLC analysis.

  5. Resolution of a disputed albendazole result in the UK Official Control System - time for more guidance?

    PubMed

    Walker, Michael; Gray, Kirstin; Hopley, Christopher; Mussell, Christopher; Clifford, Louise; Meinerikandathevan, Jayanie; Firpo, Leonardo; Topping, Joanna; Santacruz, Daniel

    2017-04-01

    Albendazole, one of the benzimidazole anthelmintics, is used in ruminants and has maximum residue limits in muscle, fat and other tissue owing to reported teratogenicity. Albendazole is extensively metabolised in domestic animals and humans with rapid conversion to a sulphoxide and subsequently sulphone and amino sulphone metabolites. Sulphoxide metabolites are responsible for the systemic biological activity of benzimidazole drugs. Herein we report a case of disputed results for albendazole in a consignment sampled at import in which the Official Analyst certified against the consignment for excess albendazole. A laboratory acting for the importer reported data below the MRL, including a finding of the parent drug which is not included in the residue definition. The Government Chemist has a statutory duty as a route of technical appeal in the UK Official Food Control system and the case was referred for referee analysis. We report our findings based on a LC-MS/MS method, which confirmed the official findings, did not reveal the presence of the parent drug but identified hot spots of albendazole marker residues in the consignment. We discuss the need for recommendations on official sampling at import and interpretation of results.

  6. 40 CFR 141.54 - Maximum residual disinfectant level goals for disinfectants.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... for disinfectants. MRDLGs for disinfectants are as follows: Disinfectant residual MRDLG(mg/L) Chlorine 4 (as Cl 2). Chloramines 4 (as Cl 2). Chlorine dioxide 0.8 (as ClO2) [63 FR 69465, Dec. 16, 1998] ...

  7. 40 CFR 141.54 - Maximum residual disinfectant level goals for disinfectants.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... for disinfectants. MRDLGs for disinfectants are as follows: Disinfectant residual MRDLG(mg/L) Chlorine 4 (as Cl 2). Chloramines 4 (as Cl 2). Chlorine dioxide 0.8 (as ClO2) [63 FR 69465, Dec. 16, 1998] ...

  8. Persistence, metabolism and safety evaluation of thiamethoxam in tomato crop.

    PubMed

    Karmakar, Rajib; Kulshrestha, Gita

    2009-08-01

    Thiamethoxam, a neonicotinoid insecticide, has been widely accepted for use in various crops, including vegetables, owing to its high efficacy against various chewing and sucking insect pests. In this particular study, the authors examined the residue dynamics of this insecticide in tomato and soil and calculated a safety index for this insecticide in an Indian context. In tomato fruits, the insecticide dissipated from 82 to 87% in 10 days with a half-life of 4 days, whereas dissipation in soil, under tomato crop, varied between 72 and 75% in 15 days with a half-life of 9 days. Total residues reached below detectable level in 15 days in tomato fruits and 20 days in soil. Maximum damage (30%) was found in control plots, as opposed to 8-10% of fruit damage in treated plots. One degradation product was detected on the tomato fruit surface, and three metabolites were identified in tomato fruits by the LC-MS technique. The metabolites have been reported for the first time in tomato fruits. Thiamethoxam at normal and double the recommended use rate effectively controlled aphids, whiteflies and Helicoverpa, as the insect population decreased to a minimum within 10 days of spraying in comparison with the control. There was no significant difference between the two rates of application, and both thiamethoxam treatments significantly increased tomato fruit yield compared with the untreated control. A maximum residue limit (MRL) of 0.05 mg kg(-1) for tomato has been proposed, with a corresponding preharvest interval (PHI) of 8 days. These parallel advances in toxicology and analytical chemistry have strengthened the observations that thiamethoxam can be used safely and efficiently in crop protection programmes.

  9. Comparative study of three screening tests, two microbiological tube tests, and a multi-sulphonamide ELISA kit for the detection of antimicrobial and sulphonamide residues in eggs.

    PubMed

    Gaudin, V; Hedou, C; Rault, A; Sanders, P; Verdon, E

    2009-04-01

    The screening of antimicrobial residues in eggs is an especially important subject. Three different commercial kits for the screening of sulphonamides and other antimicrobials in eggs were validated in accordance with Decision 2002/657/EC: one enzyme-linked immunoabsorbant assay (ELISA) kit multi-sulphonamides (from RAISIO Diagnostics) and two microbiological tests (a Premi test from DSM and an Explorer kit from Zeu-Inmunotec). The false-positive rates were lower than 2% for all kits. The detection capabilities (CCbeta) have to be as low as possible for banned substances and lower than the maximum residue limit (MRL) when MRLs have been set. The sensitivity of the Premi test was better than that of the Explorer test, probably because of the dilution of the eggs before the Explorer test was used. The CCbeta values towards most of the tested sulphonamides were satisfactory with the Premi test (< or = 100 microg kg(-1)). Performance in a proficiency test for the detection of sulphonamides in eggs with the Premi test confirmed these results. The detection capabilities of tetracycline and doxycycline were at the level of the MRL or twice the MRL maximum. The detection capabilities for chlortetracycline and oxytetracycline were higher (four to six times the MRL). The detection capabilities for amoxicillin, neomycin, tylosin and erythromycin were lower than their respective MRLs. Detection capabilities for sulphonamides were much lower for the ELISA kit than for microbiological tests. The ELISA kit could be recommended for the targeted screening of sulphonamides in eggs. On the other hand, the Explorer and Premi tests could be used as wide screening tests allowing the detection of most of the antimicrobial families.

  10. Residues of veterinary antibiotics in manures from feedlot livestock in eight provinces of China.

    PubMed

    Zhao, Ling; Dong, Yuan Hua; Wang, Hui

    2010-02-01

    The residue levels of selected fluoroquinolones, sulfonamides and tetracyclines in 143 animal dung samples collected in 2007 from large-scale livestock and poultry feedlots in 8 provinces were determined by using ultrasonic extraction and liquid chromatography. Recoveries from spiked pig dung samples (spike level=1mg/kg) ranged from 73.9 to 102.0% for fluoroquinolones, from 81.6 to 92.3% for sulfonamides, and from 57.2 to 72.6% for tetracyclines. Relative standard deviations of the recoveries were less than 10% within the same day. Method quantification limits were measured from 0.031 to 0.150 mg/kg for fluoroquinolones, from 0.023 to 0.082 mg/kg for sulfonamides, and 0.091 to 0.182 mg/kg for tetracyclines in spiked pig manure samples. Analysis of 61 pig, 54 chicken and 28 cow dung samples collected in China revealed that in pig and cow dung, up to 33.98 and 29.59 mg/kg ciprofloxacin, 33.26 and 46.70 mg/kg enrofloxacin, 59.06 and 59.59 mg/kg oxytetracycline, and 21.06 and 27.59 mg/kg chlortetracycline could be detected, respectively. A maximum concentration of 99.43 mg/kg fleroxacin, 225.45 mg/kg norfloxacin, 45.59 mg/kg ciprofloxacin and 1420.76 mg/kg enrofloxacin could be detected in chicken dung. No appreciable sulfonamide antibiotic concentrations (less than 10mg/kg) were found in any animal dung, and only sulfadimidine was observed, at a maximum concentration of 6.04 mg/kg, in chicken dung. Both enrofloxacin and chlortetracycline were detected with a very high occurrence in three animal manure samples. The residue levels for most antibiotics showed significant statistical differences among the sampling districts and the animal species. Copyright 2009 Elsevier B.V. All rights reserved.

  11. What is the relationship between free flow and pressure flow studies in women?

    PubMed

    Duckett, Jonathan; Cheema, Katherine; Patil, Avanti; Basu, Maya; Beale, Sian; Wise, Brian

    2013-03-01

    The relationship between free flow (FFS) and pressure flow (PFS) voiding studies remains uncertain and the effect of a urethral catheter on flow rates has not been determined. The relationship between residuals obtained at FF and PFS has yet to be established. This was a prospective cohort study based on 474 consecutive women undergoing cystometry using different sized urethral catheters at different centres. FFS and PFS data were compared for different conditions and the relationship of residuals analysed for FFS and PFS. The null hypothesis was that urethral catheters do not produce an alteration in maximum flow rates for PFS and FF studies. Urethral catheterisation results in lower flow rates (p < 0.01) and this finding is confirmed when flows are corrected for voided volume (p < 0.01). FFS and PFS maximum flow rates are lower in women with DO than USI (p < 0.01). A 6-F urethral catheter does not have a significantly greater effect than a 4.5-F urethral catheter. A mathematical model can be applied to transform FFS to PFS flow rates and vice versa. There was no significant difference between the mean residuals of the two groups (FFS vs PFS-two-tailed t = 0.54, p = 0.59). Positive residuals in FFS showed a good association with positive residuals in the PFS (r = 0.53, p < 0.01) Urethral catheterisation results in lower maximum flow rates. The relationship can be compared mathematically. The null hypothesis can be rejected.

  12. Bayesian image reconstruction - The pixon and optimal image modeling

    NASA Technical Reports Server (NTRS)

    Pina, R. K.; Puetter, R. C.

    1993-01-01

    In this paper we describe the optimal image model, maximum residual likelihood method (OptMRL) for image reconstruction. OptMRL is a Bayesian image reconstruction technique for removing point-spread function blurring. OptMRL uses both a goodness-of-fit criterion (GOF) and an 'image prior', i.e., a function which quantifies the a priori probability of the image. Unlike standard maximum entropy methods, which typically reconstruct the image on the data pixel grid, OptMRL varies the image model in order to find the optimal functional basis with which to represent the image. We show how an optimal basis for image representation can be selected and in doing so, develop the concept of the 'pixon' which is a generalized image cell from which this basis is constructed. By allowing both the image and the image representation to be variable, the OptMRL method greatly increases the volume of solution space over which the image is optimized. Hence the likelihood of the final reconstructed image is greatly increased. For the goodness-of-fit criterion, OptMRL uses the maximum residual likelihood probability distribution introduced previously by Pina and Puetter (1992). This GOF probability distribution, which is based on the spatial autocorrelation of the residuals, has the advantage that it ensures spatially uncorrelated image reconstruction residuals.

  13. Evaluation of ecological risk to populations of a threatened plant from an invasive biocontrol insect

    USGS Publications Warehouse

    Louda, S.M.; Rand, T.A.; Arnett, A.E.; McClay, A.S.; McEachern, A.K.

    2005-01-01

    This study was conducted to determine the influence of residues of organochlorine pollutants on reproductive success in the brown pelican. A sample egg was taken from each of 93 marked nests in the nesting colony in South Carolina. Periodic visits were made to determine the fate of marked nests. Each sample egg was analysed for residues of organochlorine pollutants. Nest success in the brown pelican was related to residues of DDE and dieldrin in sample eggs. DDE seemed primarily responsible for nest failure; however, deleterious effects of this pollutant on nest success were not satisfactorily separated from those induced by dieldrin. Significant intercorrelation of all five organochlorine residues identified in the eggs complicated the relationship of residues to nest success. Maximum DDE residues in an egg from a successful nest were 2.37 ?g/g and 8.48 ?g/g in an egg from an unsuccessful nest. Comparable maximum residues for dieldrin in sample eggs were 0.54 ?g/g (successful) and 0.99 ?g/g (unsuccessful). Nineteen of the 26 eggs from unsuccessful nests contained DDE residues that exceeded 2.37 ?g/g, and 14 of these 26 eggs contained dieldrin residues that exceeded O.54 ?g/g. Residues of DDD, DDT or PCBs in sample eggs were not significantly related to nest success. Reproductive success in the brown pelican colony was subnormal in the years of study--1971 and 1972--but reproductive success was normal in those nests in which the sample egg contained either <2,5 ?g/g of DDE or 0.54 ?g/g of dieldrin.

  14. 40 CFR 1065.720 - Liquefied petroleum gas.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ..., C3H8 Minimum, 0.85 m3/m3 ASTM D2163-05. Vapor pressure at 38 °C Maximum, 1400 kPa ASTM D1267-02 or 2598-022. Volatility residue (evaporated temperature, 35 °C) Maximum, −38 °C ASTM D1837-02a. Butanes Maximum, 0.05 m3/m3 ASTM D2163-05. Butenes Maximum, 0.02 m3/m3 ASTM D2163-05. Pentenes and heavier Maximum...

  15. Pesticide residue levels in green beans cultivated in Souss Masa valley (Morocco) after multiple applications of bifenthrin and λ-cyhalothrin.

    PubMed

    Bouri, M; Salghi, R; Bazzi, Lh; Zarrouk, A; Rios, A; Zougagh, M

    2012-09-01

    Dissipation of bifenthrin and λ-cyhalothrin pyrethroid insecticides, under environmental conditions, was evaluated on green beans grown in experimental greenhouses (Souss Massa valley, Morocco). Pesticide residues were determined by gas chromatography with micro electron-capture detector (GC-μECD) after dichloromethane extraction and cleanup on florisil phase cartridges. In the case of field experiments, a random block scheme was employed. Each block contained 25 plants in a single row and tests were carried out in triplicates applying pesticides at the recommended doses by the manufacturers. Fruit samples were periodically taken until the end of the preharvest interval (p.i.). The results obtained showed that the p.i of bifenthrin in green bean were 4 days in the winter and 3.5 days in the spring, whereas that for λ-cyhalothrin 8 days was found in the winter and 7.5 days in the spring. Consequently, it is possible to consider the European Union maximum residue limit (EU MRL) values compatible with the proper agricultural practices used for growing green bean in the plastic greenhouse of Souss Massa valley in South Morocco. Bifenthrin had a degradation of first-order kinetics, whereas that of levels for λ-cyhalothrin residue can not be interpreted by the use of a first order model.

  16. Behavior of pesticides in coffee beans during the roasting process.

    PubMed

    Sakamoto, Katsushi; Nishizawa, Hideo; Manabe, Noboru

    2012-01-01

    In Japan, maximum residue limits for pesticides (MRL) in coffee are set on green coffee beans, but not roasted coffee beans, although roasted beans are actually used to prepare coffee for drinking. Little is known about the behavior of pesticides during the roasting process. In the present study, we examined the changes in the concentration of pesticide (organochlorine: γ-BHC, chlordane and heptachlor) residues in coffee beans during the roasting process. We prepared green coffee beans spiked with these pesticides (0.2 and 1.0 μg/g), and the residue levels in the beans were measured before and after the roasting process. We determined the residual rate after the roasting process. γ-BHC was not detectable at all, and more than 90% of chlordane was lost after the roasting (3.1 and 5.1% of chlordane remained in the beans spiked with 0.2 and 1.0 μg/g of chlordane, respectively). A low level of heptachlor (0.72%) was left in the coffee beans spiked with 1 μg/g of heptachlor. Disappearance of γ-BHC during the roasting process may be due to the high vapor pressure of γ-BHC, while chlordane has a lower vapor pressure. We also examined the behavior of piperonyl butoxide and atrazine during the roasting process. Piperonyl butoxide behaved similarly to chlordane, but atrazine disappeared after the roasting process, because it is unstable to heat.

  17. Quantitative spatial frequency fluorescence imaging in the sub-diffusive domain for image-guided glioma resection

    PubMed Central

    Sibai, Mira; Veilleux, Israel; Elliott, Jonathan T.; Leblond, Frederic; Wilson, Brian C.

    2015-01-01

    Intraoperative 5- aminolevulinic acid induced-Protoporphyrin IX (PpIX) fluorescence guidance enables maximum safe resection of glioblastomas by providing surgeons with real-time tumor optical contrast. However, visual assessment of PpIX fluorescence is subjective and limited by the distorting effects of light attenuation and tissue autofluorescence. We have previously shown that non-invasive point measurements of absolute PpIX concentration identifies residual tumor that is otherwise non-detectable. Here, we extend this approach to wide-field quantitative fluorescence imaging by implementing spatial frequency domain imaging to recover tissue optical properties across the field-of-view in phantoms and ex vivo tissue. PMID:26713206

  18. Mechanical properties of high-temperature superconducting wires. Ph.D. Thesis - Illinois Inst. of Tech.

    NASA Technical Reports Server (NTRS)

    Goretta, K. C.; Cluff, J. A.; Joo, J.; Lanagan, M. T.; Singh, J. P.; Vasanthamohan, N.; Xin, Y.; Wong, K. W.

    1995-01-01

    Bending strength, fracture toughness, and elastic modulus data were acquired for YBa2Cu3O(x), Bi2Sr2CaCu2O(x) (Bi,Pb)2Sr2Ca2Cu3O(x), and Tl2Ba2Ca2Cu3O(x) bars. These data and thermal expansion coefficients strongly suggest that the maximum possible tensile strain without fracture of bulk tapes or wires is approximately equals 0.2%. In Ag-clad conductors, residual stresses will be of limited benefit, but fractures produced by larger strains can be accommodated by shunting current through the Ag.

  19. 40 CFR 141.60 - Effective dates.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS National Primary Drinking Water Regulations: Maximum Contaminant Levels and Maximum Residual Disinfectant Levels § 141.60 Effective dates. (a) The effective dates for § 141...

  20. Aluminum-thin-film packaged fiber Bragg grating probes for monitoring the maximum tensile strain of composite materials.

    PubMed

    Im, Jooeun; Kim, Mihyun; Choi, Ki-Sun; Hwang, Tae-Kyung; Kwon, Il-Bum

    2014-06-10

    In this paper, new fiber Bragg grating (FBG) sensor probes are designed to intermittently detect the maximum tensile strain of composite materials, so as to evaluate the structural health status. This probe is fabricated by two thin Al films bonded to an FBG optical fiber and two supporting brackets, which are fixed on the surface of composite materials. The residual strain of the Al packaged FBG sensor probe is induced by the strain of composite materials. This residual strain can indicate the maximum strain of composite materials. Two types of sensor probes are prepared-one is an FBG with 18 μm thick Al films, and the other is an FBG with 36 μm thick Al films-to compare the thickness effect on the detection sensitivity. These sensor probes are bonded on the surfaces of carbon fiber reinforced plastics composite specimens. In order to determine the strain sensitivity between the residual strain of the FBG sensor probe and the maximum strain of the composite specimen, tensile tests are performed by universal testing machine, under the loading-unloading test condition. The strain sensitivities of the probes, which have the Al thicknesses of 18 and 36 μm, are determined as 0.13 and 0.23, respectively.

  1. Uptake of organochlorine pesticides by zucchini cultivars grown in polluted soils.

    PubMed

    Donnarumma, L; Pompi, V; Faraci, A; Conte, E

    2008-01-01

    Aim of this trial was to verify the occurrence and the distribution of organochlorine pesticides (OCPs) in zucchini cultivated varieties grown in glasshouses and in open field with different levels of pollutants in soil. Residues of OCPs have been detected in soils and crops in the province of Latina, an intensively agricultural area of Lazio Region, in Italy. The study has been focused at crop harvest in less contaminated glasshouses and during crop life cycle in contaminated field in spring-summer time. Dieldrin distribution in different part of plant is similar among zucchini cultivars grown in contaminated field. In crop grown in field and in glasshouses with soil pollution >0.01 mg/kg, we found dieldrin in all zucchini fruits and flowers, at the same level or higher than the maximum residue limit (RML) fixed by European law for edible vegetables (0.02 mg/kg). Instead in soil with pollution < or = 0.01 mg/kg total OCPs it would be possible to grow zucchini cultivars.

  2. Design and characterization of a microbial fuel cell for the conversion of a lignocellulosic crop residue to electricity.

    PubMed

    Gregoire, K P; Becker, J G

    2012-09-01

    Agricultural crop residues contain high amounts of biochemical energy as cellulose and lignin. A portion of this biomass could be sustainably harvested for conversion to bioenergy to help offset fossil fuel consumption. In this study, the potential for converting lignocellulosic biomass directly to electricity in a microbial fuel cell (MFC) was explored. Design elements of tubular air cathode MFCs and leach-bed bioreactors were integrated to develop a new solid-substrate MFC in which cellulose hydrolysis, fermentation, and anode respiration occurred in a single chamber. Electricity was produced continuously from untreated corncob pellets for >60 d. Addition of rumen fluid increased power production, presumably by providing growth factors to anode-respiring bacteria. Periodic exposure to oxygen also increased power production, presumably by limiting the diversion of electrons to methanogenesis. In the absence of methanogenesis, bioaugmentation with Geobacter metallireducens further improved MFC performance. Under these conditions, the maximum power density was 230 mW/m(3). Copyright © 2012 Elsevier Ltd. All rights reserved.

  3. Dissipation Pattern, Processing Factors, and Safety Evaluation for Dimethoate and Its Metabolite (Omethoate) in Tea (Camellia Sinensis).

    PubMed

    Pan, Rong; Chen, Hong-Ping; Zhang, Ming-Lu; Wang, Qing-Hua; Jiang, Ying; Liu, Xin

    2015-01-01

    Residue levels of dimethoate and its oxon metabolite (omethoate) during tea planting, manufacturing, and brewing were investigated using a modified QuEChERS sample preparation and gas chromatography. Dissipation of dimethoate and its metabolite in tea plantation followed the first-order kinetic with a half-life of 1.08-1.27 d. Tea manufacturing has positive effects on dimethoate dissipation. Processing factors of dimethoate are in the range of 2.11-2.41 and 1.41-1.70 during green tea and black tea manufacturing, respectively. Omethoate underwent generation as well as dissipation during tea manufacturing. Sum of dimethoate and omethoate led to a large portion of 80.5-84.9% transferring into tea infusion. Results of safety evaluation indicated that omethoate could bring higher human health risk than dimethoate due to its higher hazard quotient by drinking tea. These results would provide information for the establishment of maximum residue limit and instruction for the application of dimethoate formulation on tea crop.

  4. Quantitative analysis of fungicide azoxystrobin in agricultural samples with rapid, simple and reliable monoclonal immunoassay.

    PubMed

    Watanabe, Eiki; Miyake, Shiro

    2013-01-15

    This work presents analytical performance of a kit-based direct competitive enzyme-linked immunosorbent assay (dc-ELISA) for azoxystrobin detection in agricultural products. The dc-ELISA was sufficiently sensitive for analysis of residue levels close to the maximum residue limits. The dc-ELISA did not show cross-reactivity to other strobilurin analogues. Absorbance decreased with the increase of methanol concentration in sample solution from 2% to 40%, while the standard curve became most linear when the sample solution contained 10% methanol. Agricultural samples were extracted with methanol, and the extracts were diluted with water to 10% methanol adequate. No significant matrix interference was observed. Satisfying recovery was found for all of spiked samples and the results were well agreed with the analysis with liquid chromatography. These results clearly indicate that the kit-based dc-ELISA is suitable for the rapid, simple, quantitative and reliable determination of the fungicide. Copyright © 2012 Elsevier Ltd. All rights reserved.

  5. Use of body plethysmography to measure effect of bimaxillary orthognathic surgery on airway resistance and lung volumes.

    PubMed

    Rezaeetalab, Fariba; Kazemian, Mozhgan; Vaezi, Touraj; Shaban, Barratollah

    2015-12-01

    Bimaxillary orthognathic surgery can cause changes to respiration and the airways. We used body plethysmography to evaluate its effect on airway resistance and lung volumes in 20 patients with class III malocclusions (8 men and 12 women, aged 17 - 32 years). Lung volumes (forced vital capacity; forced inspiratory volume/one second; forced expiratory volume/one second: forced vital capacity; peak expiratory flow; maximum expiratory flow 25-75; maximum inspiratory flow; total lung capacity; residual volume; residual volume:total lung capacity), and airway resistance were evaluated one week before, and six months after, operation. Bimaxillary operations to correct class III malocclusions significantly increased airway resistance, residual volume, total lung capacity, and residual volume:total lung capacity. Other variables also changed after operation but not significantly so. Orthognathic operations should be done with caution in patients who have pre-existing respiratory diseases. Copyright © 2015 The British Association of Oral and Maxillofacial Surgeons. Published by Elsevier Ltd. All rights reserved.

  6. Development and validation of a general derivatization HPLC method for the trace analysis of acyl chlorides in lipophilic drug substances.

    PubMed

    Zheng, Xiangyuan; Luo, Lan; Zhou, Jie; Ruan, Xiaoling; Liu, Wenyuan; Zheng, Feng

    2017-06-05

    Acyl chlorides are important acylating agents in the synthesis of active pharmaceutical ingredients. Determining the residual acyl chlorides in drug substances is a challenge due to their high reactivity and the matrix interferences from drug substances and their related impurities. This paper describes a general derivatization HPLC method for the determination of aromatic and aliphatic acyl chlorides in lipophilic drug substances. Since most drug substances have weak absorptions in the visible range (above 380nm), the nitro-substituted anilines and nitro-substituted phenylhydrazines were selected as the derivatization reagents due to their weak basicity and red-shift of UV absorption spectra. The maximum wavelength and absorption intensity of nitro-substituted anilines decreased after derivatization with acyl chlorides, whereas the derivatization products of nitro-substituted phenylhydrazines showed the slight increases of maximum wavelength and absorbance intensity. Hence, 2-nitrophenylhydrazine was selected as the suitable derivatization reagent because the derivatives have the maximum UV wavelength absorbance at 395nm, which could largely minimize the matrix interferences. The optimization of the concentration of 2-nitrophenylhydrazine is important for the sensitivity and stability of derivatives. Other reaction conditions including reaction temperature, time and the influence of three competitive solvents (water, methanol and ethanol) on the reaction efficiency were also studied. After derivatization with 100μgmL -1 2-nitrophenylhydrazine at room temperature for 30min, the method was validated for high specificity and sensitivity with the detection limits in the range of 0.01-0.03μgmL -1 . The proposed method was applied as a generic method to determine the residual acyl chlorides in lipophilic drug substances. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Concentrations and dissipation of difenoconazole and fluxapyroxad residues in apples and soil, determined by ultrahigh-performance liquid chromatography electrospray ionization tandem mass spectrometry.

    PubMed

    He, Min; Jia, Chunhong; Zhao, Ercheng; Chen, Li; Yu, Pingzhong; Jing, Junjie; Zheng, Yongquan

    2016-03-01

    A new combined difenoconazole and fluxapyroxad fungicide formulation, as an 11.7 % suspension concentrate (SC), has been introduced as part of a resistance management strategy. The dissipation of difenoconazole and fluxapyroxad applied to apples and the residues remaining in the apples were determined. The 11.7 % SC was sprayed onto apple trees and soil in Beijing, Shandong, and Anhui provinces, China, at an application rate of 118 g a.i. ha(-1), then the dissipation of difenoconazole and fluxapyroxad was monitored. The residual difenoconazole and fluxapyroxad concentrations were determined by ultrahigh-performance liquid chromatography tandem mass spectrometry. The difenoconazole half-lives in apples and soil were 6.2-9.5 and 21.0-27.7 days, respectively. The fluxapyroxad half-lives in apples and soil were 9.4-12.6 and 10.3-36.5 days, respectively. Difenoconazole and fluxapyroxad residues in apples and soil after the 11.7 % SC had been sprayed twice and three times, with 10 days between applications, at 78 and 118 g a.i. ha(-1) were measured. Representative apple and soil samples were collected after the last treatment, at preharvest intervals of 14, 21, and 28 days. The difenoconazole residue concentrations in apples and soil were 0.002-0.052 and 0.002-0.298 mg kg(-1), respectively. The fluxapyroxad residue concentrations in apples and soil were 0.002-0.093 and 0.008-1.219 mg kg(-1), respectively. The difenoconazole and fluxapyroxad residue concentrations in apples were lower than the maximum residue limits (0.5 and 0.8 mg kg(-1), respectively). An application rate of 78 g a.i. ha(-1) is therefore recommended to ensure that treated apples can be considered safe for humans to consume.

  8. Computer-aided Assessment of Regional Abdominal Fat with Food Residue Removal in CT

    PubMed Central

    Makrogiannis, Sokratis; Caturegli, Giorgio; Davatzikos, Christos; Ferrucci, Luigi

    2014-01-01

    Rationale and Objectives Separate quantification of abdominal subcutaneous and visceral fat regions is essential to understand the role of regional adiposity as risk factor in epidemiological studies. Fat quantification is often based on computed tomography (CT) because fat density is distinct from other tissue densities in the abdomen. However, the presence of intestinal food residues with densities similar to fat may reduce fat quantification accuracy. We introduce an abdominal fat quantification method in CT with interest in food residue removal. Materials and Methods Total fat was identified in the feature space of Hounsfield units and divided into subcutaneous and visceral components using model-based segmentation. Regions of food residues were identified and removed from visceral fat using a machine learning method integrating intensity, texture, and spatial information. Cost-weighting and bagging techniques were investigated to address class imbalance. Results We validated our automated food residue removal technique against semimanual quantifications. Our feature selection experiments indicated that joint intensity and texture features produce the highest classification accuracy at 95%. We explored generalization capability using k-fold cross-validation and receiver operating characteristic (ROC) analysis with variable k. Losses in accuracy and area under ROC curve between maximum and minimum k were limited to 0.1% and 0.3%. We validated tissue segmentation against reference semimanual delineations. The Dice similarity scores were as high as 93.1 for subcutaneous fat and 85.6 for visceral fat. Conclusions Computer-aided regional abdominal fat quantification is a reliable computational tool for large-scale epidemiological studies. Our proposed intestinal food residue reduction scheme is an original contribution of this work. Validation experiments indicate very good accuracy and generalization capability. PMID:24119354

  9. Computer-aided assessment of regional abdominal fat with food residue removal in CT.

    PubMed

    Makrogiannis, Sokratis; Caturegli, Giorgio; Davatzikos, Christos; Ferrucci, Luigi

    2013-11-01

    Separate quantification of abdominal subcutaneous and visceral fat regions is essential to understand the role of regional adiposity as risk factor in epidemiological studies. Fat quantification is often based on computed tomography (CT) because fat density is distinct from other tissue densities in the abdomen. However, the presence of intestinal food residues with densities similar to fat may reduce fat quantification accuracy. We introduce an abdominal fat quantification method in CT with interest in food residue removal. Total fat was identified in the feature space of Hounsfield units and divided into subcutaneous and visceral components using model-based segmentation. Regions of food residues were identified and removed from visceral fat using a machine learning method integrating intensity, texture, and spatial information. Cost-weighting and bagging techniques were investigated to address class imbalance. We validated our automated food residue removal technique against semimanual quantifications. Our feature selection experiments indicated that joint intensity and texture features produce the highest classification accuracy at 95%. We explored generalization capability using k-fold cross-validation and receiver operating characteristic (ROC) analysis with variable k. Losses in accuracy and area under ROC curve between maximum and minimum k were limited to 0.1% and 0.3%. We validated tissue segmentation against reference semimanual delineations. The Dice similarity scores were as high as 93.1 for subcutaneous fat and 85.6 for visceral fat. Computer-aided regional abdominal fat quantification is a reliable computational tool for large-scale epidemiological studies. Our proposed intestinal food residue reduction scheme is an original contribution of this work. Validation experiments indicate very good accuracy and generalization capability. Published by Elsevier Inc.

  10. Residue levels and risk assessment of pesticides in nuts of China.

    PubMed

    Liu, Yihua; Shen, Danyu; Li, Shiliang; Ni, Zhanglin; Ding, Ming; Ye, Caifen; Tang, Fubin

    2016-02-01

    The pesticide residue levels of three nuts (chestnut, walnut, pinenut) collected from seven main producing areas of China were investigated. Twenty-nine pesticides, including organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and two fungicides (triadimefon and buprofezin) were analyzed by gas chromatography (GC). Four OPs (acephate, dimethoate, chlorpyrifos and parathion-methyl) were found in 11.4% samples, with the concentrations of 19.0 µg kg(-1) to 74.0 µg kg(-1). Six OCs (DDT, HCH, endosulfan, quintozene, aldrin and dieldrin) were found in 18.2% samples, with the concentrations of 2.0 µg kg(-1) to 65.7 µg kg(-1). Among OCs, p,p-DDE and α-HCH were the dominant isomer for DDT and HCH. Five PYs (fenpropathrin, fenvalerate, cypermethrin, bifenthrin and cyhalothrin) were found in 15.9% samples, with the concentrations of 2.5 µg kg(-1) to 433.0 µg kg(-1). Fenpropathrin was the most frequently detected pesticide. In addition, triadimefon and buprofezin were detected only in two samples. For the tested nuts, 25.0% samples with multiple residues (containing more than two pesticides) were noted, even up to 9.1% samples with five pesticide residues. The residue of 15.9% samples was higher than the maximum residue limits (MRLs) of China. The short-term risks for the tested nuts were below 1.2%, and the highest long-term risk was 12.58%. The cumulative risk (cHI) for the tested pesticides were 8.43% (OPs), 0.42% (OCs), 12.82% (PYs) and 0.15% (fungicides), respectively. The total cHI was 21.82%. There was no significant health risk for consumers via nuts consumption. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Extraction of manganese from electrolytic manganese residue by bioleaching.

    PubMed

    Xin, Baoping; Chen, Bing; Duan, Ning; Zhou, Changbo

    2011-01-01

    Extraction of manganese from electrolytic manganese residues using bioleaching was investigated in this paper. The maximum extraction efficiency of Mn was 93% by sulfur-oxidizing bacteria at 4.0 g/l sulfur after bioleaching of 9days, while the maximum extraction efficiency of Mn was 81% by pyrite-leaching bacteria at 4.0 g/l pyrite. The series bioleaching first by sulfur-oxidizing bacteria and followed by pyrite-leaching bacteria evidently promoted the extraction of manganese, witnessing the maximum extraction efficiency of 98.1%. In the case of sulfur-oxidizing bacteria, the strong dissolution of bio-generated sulfuric acid resulted in extraction of soluble Mn2+, while both the Fe2+ catalyzed reduction of Mn4+ and weak acidic dissolution of Mn2+ accounted for the extraction of manganese with pyrite-leaching bacteria. The chemical simulation of bioleaching process further confirmed that the acid dissolution of Mn2+ and Fe2+ catalyzed reduction of Mn4+ were the bioleaching mechanisms involved for Mn extraction from electrolytic manganese residues. Copyright © 2010 Elsevier Ltd. All rights reserved.

  12. Comparison of the composting process using ear corn residue and three other conventional bulking agents during cow manure composting under high-moisture conditions.

    PubMed

    Hanajima, Dai

    2014-10-01

    To elucidate the characteristics of ear corn residue as a bulking agent, the composting process using this residue was compared with processes using three other conventional materials such as sawdust, wheat straw and rice husk, employing a bench-scale composting reactor. As evaluated via biochemical oxygen demand (BOD), ear corn residue contains 3.3 and 2.0 times more easily digestible materials than sawdust and rice husk, respectively. In addition, mixing ear corn residue with manure resulted in reduced bulk density, which was the same as that of wheat straw and was 0.58 and 0.67 times lower than that of sawdust and a rice husk mixture, respectively. To evaluate temperature generation during the composting process, the maximum temperature and area under the temperature curve (AUCTEMP) were compared among the mixed composts of four bulking agents. Maximum temperature (54.3°C) as well as AUCTEMP (7310°C●h) of ear corn residue were significantly higher than those of sawdust and rice husk (P<0.05), and they are similar to that of wheat straw mixed compost. Along with the value of AUCTEMP, the highest organic matter losses of 31.1% were observed in ear corn residue mixed compost, followed by wheat straw, saw dust and rice husk. © 2014 Japanese Society of Animal Science.

  13. Occurrence of pesticide residues in fruiting vegetables from production farms in south-eastern region of Poland

    PubMed

    Słowik-Borowiec, Magdalena; Szpyrka, Ewa; Rupar, Julian; Podbielska, Magdalena; Matyaszek, Aneta

    Considering the fact that pesticides are commonly used in agriculture, continuous monitoring of these substances in food products is of great significance. Residues of these substances can be present in crops after harvest. The aim of this study was to evaluate presence of pesticide residues in fruiting vegetables from production farms in south-eastern region of Poland in 2012–2015. 138 samples were tested using accredited test methods. The monitoring programme covered determination of 242 pesticides. The tests covered tomato, cucumber and pepper crops. The test results were interpreted in accordance with criteria included in the European Commission recommendations published in the document SANCO/12571/2013 (now superseded by Document SANTE 2015), as well as on a basis of the maximum residue levels in force in the EU Member States. Pesticide residues were found in 47 samples, representing 34% of all tested samples. 17 active substances were found, belonging to fungicides and insecticides. Azoxystrobin (38%), boscalid (28%) and chlorothalonil (21%) were most commonly found in fruiting vegetables testing samples. Non-compliances related to use of plant protection product not authorized for protection of a given crop were observed in 6% of analysed samples. However, pesticide residues of fruiting vegetables in quantities that exceed the maximum residue levels (NDP, ang. MRLs), as well as substances which use for plant protection is forbidden were no found. Crops monitoring is used to determine to what extent such products are contaminated with pesticide residues, and ensures protection of customer health.

  14. Analysis of Risks to Oxygen Systems from Particulate and Fiber Contaminants and Derivation of Cleanliness Requirements

    NASA Technical Reports Server (NTRS)

    Lowrey, Nikki M.

    2016-01-01

    It has been well documented in the literature that contamination within oxygen systems can create significant fire hazards. Cleanliness limits for nonvolatile residues, ranging from 10 to 500 milligrams per square meter, have been established for various industries and types of oxygen systems to reduce the risk of ignition of flammable organic films. Particulate cleanliness limits used for oxygen systems, however, vary considerably, notably within the aerospace industry. Maximum allowed particle size, quantity limits, and allocations for fibers or metallic particles are all variables seen in aerospace cleanliness limits. Particles are known to have the potential to ignite within oxygen systems and must be limited to prevent fires. Particulate contamination may also pose risks to the performance of oxygen systems that are unrelated to ignition hazards. An extensive literature search was performed to better understand the relative importance of particle ignition mechanisms versus other deleterious effects of particles on oxygen systems and to identify rationale for derivation of particulate cleanliness limits for specific systems. The identified risks of different types and sizes of particles and fibers were analyzed. This paper summarizes the risks identified and rationale that may be used to derive particulate cleanliness limits for specific oxygen systems.

  15. Analysis of Risks to Oxygen Systems from Particulate and Fiber Contaminants and Derivation of Cleanliness Requirements

    NASA Technical Reports Server (NTRS)

    Lowrey, Nikki M.

    2016-01-01

    It has been well documented in the literature that contamination within oxygen systems can create significant fire hazards. Cleanliness limits for nonvolatile residues, ranging from 10 to 500 mg/sq m, have been established for various industries and types of oxygen systems to reduce the risk of ignition of flammable organic films. Particulate cleanliness limits used for oxygen systems vary considerably. Maximum allowed particle size, quantity limits, and allocations for fibers or metallic particles are all variables seen in aerospace cleanliness limits. Particles are known to have the potential to ignite within oxygen systems and must be limited to prevent fires. Particulate contamination may also pose risks to the performance of oxygen systems that are unrelated to ignition hazards. An extensive literature search was performed to better understand the relative importance of particle ignition mechanisms versus other deleterious effects of particles on oxygen systems and to identify rationale for derivation of particulate cleanliness limits for specific systems. The identified risks of different types and sizes of particles and fibers were analyzed. This paper summarizes the risks identified and rationale that may be used to derive particulate cleanliness limits for specific oxygen systems.

  16. 7 CFR 58.140 - Field service.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... each producer whose milk tests positive for drug residue, exceeds the maximum somatic cell count level... milk and eliminate any potential causes of drug residues. A representative of the plant should routinely visit each producer as often as necessary to assist and encourage the production of high quality...

  17. 7 CFR 58.140 - Field service.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... each producer whose milk tests positive for drug residue, exceeds the maximum somatic cell count level... milk and eliminate any potential causes of drug residues. A representative of the plant should routinely visit each producer as often as necessary to assist and encourage the production of high quality...

  18. 7 CFR 58.140 - Field service.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... each producer whose milk tests positive for drug residue, exceeds the maximum somatic cell count level... milk and eliminate any potential causes of drug residues. A representative of the plant should routinely visit each producer as often as necessary to assist and encourage the production of high quality...

  19. 7 CFR 58.140 - Field service.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... each producer whose milk tests positive for drug residue, exceeds the maximum somatic cell count level... milk and eliminate any potential causes of drug residues. A representative of the plant should routinely visit each producer as often as necessary to assist and encourage the production of high quality...

  20. 7 CFR 58.140 - Field service.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... each producer whose milk tests positive for drug residue, exceeds the maximum somatic cell count level... milk and eliminate any potential causes of drug residues. A representative of the plant should routinely visit each producer as often as necessary to assist and encourage the production of high quality...

  1. Screening of veterinary drug residues in food by LC-MS/MS. Background and challenges.

    PubMed

    Delatour, Thierry; Racault, Lucie; Bessaire, Thomas; Desmarchelier, Aurélien

    2018-04-01

    Regulatory agencies and government authorities have established maximum residue limits (MRL) in various food matrices of animal origin for supporting governments and food operators in the monitoring of veterinary drug residues in the food chain, and ultimately in the consumer's plate. Today, about 200 veterinary drug residues from several families, mainly with antibiotic, antiparasitic or antiinflammatory activities, are regulated in a variety of food matrices such as milk, meat or egg. This article provides a review of the regulatory framework in milk and muscle including data from Codex Alimentarius, Europe, the U.S.A., Canada and China for about 220 veterinary drugs. The article also provides a comprehensive overview of the challenge for food control, and emphasizes the pivotal role of liquid chromatography-mass spectrometry (LC-MS), either in tandem with quadrupoles (LC-MS/MS) or high resolution MS (LC-HRMS), for ensuring an adequate consumer protection combined with an affordable cost. The capability of a streamlined LC-MS/MS platform for screening 152 veterinary drug residues in a broad range of raw materials and finished products is highlighted in a production line perspective. The rationale for a suite of four methods intended to achieve appropriate performance in terms of scope and sensitivity is presented. Overall, the platform encompasses one stream for the determination of 105 compounds in a run (based on acidic QuEChERS-like), plus two streams for 23 β-lactams (alkaline QuEChERS-like) and 10 tetracyclines (low-temperature partitioning), respectively, and a dedicated stream for 14 aminoglycosides (molecularly-imprinted polymer).

  2. Determination of ethoxyquin by high-performance liquid chromatography with fluorescence detection and its application to the survey of residues in food products of animal origin.

    PubMed

    Aoki, Yoichi; Kotani, Akira; Miyazawa, Naomi; Uchida, Kazunari; Igarashi, Yu; Hirayama, Norio; Hakamata, Hideki; Kusu, Fumiyo

    2010-01-01

    An analytical method using HPLC with fluorescence detection (HPLC-FL) has been developed and applied for the survey of residue levels of ethoxyquin in a variety of food products of animal origin. HPLC was performed using a silica octadecylsilane column, butylhydroxytoluene-acetonitrile-water (0.05 + 800 + 200, v/v/v) mobile phase, and detection at excitation and emission wavelengths of 370 and 415 nm, respectively. HPLC/MS was used to confirm whether a chromatographic peak was ethoxyquin. The LOQ of the foods was 0.01 microg/g, except for pig fat and cow's milk, and the RSD (n=6) at 0.1 microg/mL of the standard solution was 1.12%. The accuracy of the calculated data of the standard solution was within the range of 94.0 to 101.2%. Recoveries of ethoxyquin from the food products of cattle, pigs, chickens, and salmon were more than 71.0% with an RSD of < 9.3%, except for chicken liver at different concentration levels, including the lower LOQ, the maximum residue limit (MRL), and in some tissues, twice the MRL. Residue levels of ethoxyquin in 33 commercially available food products of animal origin that were purchased on the west side of the Tokyo metropolitan area were surveyed. Contents of ethoxyquin residues in three chicken fat samples by the HPLC-FL method were 0.08, 0.03, and 0.04 microg/g, all less than the MRL (5 microg/g).

  3. High performance liquid chromatography for the simultaneous analysis of penicillin residues in beef and milk using ion-paired extraction and binary water-acetonitrile mixture.

    PubMed

    Kukusamude, Chunyapuk; Burakham, Rodjana; Chailapakul, Orawon; Srijaranai, Supalax

    2012-04-15

    An ion-paired extraction (IPE) has been developed for the analysis of penicillin antibiotics (penicillin G, oxacillin and cloxacillin) in beef and milk samples using tetrabutylammonium bromide (TBABr) as ion-pairing agent and binary water-acetonitrile as extractant. The factors affecting the IPE efficiency were optimized including solution pH, volume of acetonitrile (ACN), concentration of TBABr and electrolyte salt (NH(4))(2)SO(4). The optimum IPE conditions were 10 mmol L(-1) phosphate buffer pH 8, 2 mL of ACN, 6 mmol L(-1) of TBABr and 2.5 mL of saturated ammonium sulfate. Under the HPLC condition: an Xbridge™ C18 reversed-phase column, isocratic elution of 5 mmol L(-1) phosphate buffer (pH 6.6) and acetonitrile (75:25, v/v) and a flow rate of 1 mL min(-1), with UV detection at 215 nm, the separation of three penicillins was achieved within 10 min. Under the selected optimum conditions, the enhancement of 21-53 folds compared to that without preconcentration and limits of detection (LODs) of 1-2 ng mL(-1) were obtained. Good reproducibility was achieved with RSD<2% for retention time and <5% for slope of calibration curves. The average recoveries higher than 85% were obtained. The proposed IPE-HPLC method has shown to be high efficient preconcentration and analysis method for penicillin residues in beef and milk with LOD lower than the maximum residue limits. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Development of a novel genetically modified bioluminescent-bacteria-based assay for detection of fluoroquinolones in animal-derived foods.

    PubMed

    Cheng, Guyue; Dong, Xiaobing; Wang, Yulian; Peng, Dapeng; Wang, Xu; Hao, Haihong; Xie, Shuyu; Qu, Wei; Liu, Zhenli; Yuan, Zonghui

    2014-12-01

    Fluoroquinolones (FQNs) are broad-spectrum antibacterial agents widely used in animal husbandry and aquaculture. The residues and antimicrobial resistance of such antibiotics are a major public health concern. To realize multianalyte detection of FQN residues, a genetically modified bacterium, Escherichia coli pK12 harboring plasmid pRecAlux3, was constructed in this study to develop a bioluminescent-bacteria-based assay for the detection of FQNs in animal-derived foods. This assay was based on the principle of induction of an SOS response by FQNs via inducing the recA-promoter-fused luciferase reporter gene existing on the plasmid pRecAlux3. E. coli pK12 was able to recognize 11 FQNs: difloxacin, enrofloxacin, ciprofloxacin, sarafloxacin, norfloxacin, danofloxacin, ofloxacin, pefloxacin, lomefloxacin, marbofloxacin, and orbifloxacin. This method could be applied to 11 edible tissues, including milk, fish muscle, and the muscles, livers, and kidneys of cattle, chickens, and pigs, with a very simple and rapid sample extraction procedure using only phosphate-buffered saline. The limits of detection of the FQNs were between 12.5 and 100 μg kg(-1), all of which were lower than the maximum residue limits. Most of the recoveries of the FQNs were in the range from 60 to 120 %, and the interassay coefficients of variation were less than 30 %. This method, confirmed by high-performance liquid chromatography, is reliable and can be used as both a screening test and a semiquantitative assay, when the identity of a single type of FQN is known.

  5. Determination of benzimidazole anthelmintics in animal-derived biological matrices.

    PubMed

    Neri, Bruno; Bidolli, Gentilina; Felli, Marialinda; Cozzani, Roberto

    2002-04-01

    This paper describes an easy multiresidue procedure for the determination of 8 benzimidazole anthelmintics (Albendazole, Albendazole sulphone, Albendazole sulphoxide, Ox-bendazole, Ossibendazole, p-OH-Fenbendazole, Fenbendazole, Flubendazole) in foodstuffs of animal origin for human consumption. According to the proposed procedure, 10 g of homogenised sample were extracted with acetonitrile in ultrasonic bath, the organic layer was evaporated to dryness and the residue dissolved in HCl 0.005 M. After an initial washing with hexane to remove fats, the aqueous layer was purified on SPE C2 column and the analytes were eluted with methanol, evaporated to dryness and reconstituted with phosphate buffer/acetonitrile (50/50). The solution obtained was analysed by HPLC with diode array detector (DAD); this detector provides useful information about the peaks present in routine samples, because it gains not only retention times of analytes, as well as their UV-spectra. Benzthiazuron was used as internal standard and the method was validated in the range 10-100 ppb, as requested by the imposed limits. The mean recoveries in spiked samples ranged between 70% and 95%, for 10 and 100 ppb respectively. The developed method resulted sensitive, simple and fast. It is particularly suitable for laboratories that execute screening analysis on a great number of samples, observing the EC regulations that establish the benzimidazole Maximum Residue Limits (MRLs) in food.

  6. Robust experimental design for optimizing the microbial inhibitor test for penicillin detection in milk.

    PubMed

    Nagel, O G; Molina, M P; Basílico, J C; Zapata, M L; Althaus, R L

    2009-06-01

    To use experimental design techniques and a multiple logistic regression model to optimize a microbiological inhibition test with dichotomous response for the detection of Penicillin G in milk. A 2(3) x 2(2) robust experimental design with two replications was used. The effects of three control factors (V: culture medium volume, S: spore concentration of Geobacillus stearothermophilus, I: indicator concentration), two noise factors (Dt: diffusion time, Ip: incubation period) and their interactions were studied. The V, S, Dt, Ip factors and V x S, V x Ip, S x Ip interactions showed significant effects. The use of 100 microl culture medium volume, 2 x 10(5) spores ml(-1), 60 min diffusion time and 3 h incubation period is recommended. In these elaboration conditions, the penicillin detection limit was of 3.9 microg l(-1), similar to the maximum residue limit (MRL). Of the two noise factors studied, the incubation period can be controlled by means of the culture medium volume and spore concentration. We were able to optimize bioassays of dichotomous response using an experimental design and logistic regression model for the detection of residues at the level of MRL, aiding in the avoidance of health problems in the consumer.

  7. Dietary risk assessment of pesticides from vegetables and drinking water in gardening areas in Burkina Faso.

    PubMed

    Lehmann, Edouard; Turrero, Nuria; Kolia, Marius; Konaté, Yacouba; de Alencastro, Luiz Felippe

    2017-12-01

    Vegetables and water samples have been collected around the lake of Loumbila in Burkina Faso. Pesticides residues in food commodities were analyzed using a modified QuEChERS extraction method prior analysis on GC-MS and UPLC-MS/MS of 31 pesticides. Maximum Residue Limits (MRLs) were exceeded in 36% of the samples for seven pesticides: acetamiprid, carbofuran, chlorpyrifos, lambda-cyhalothrin, dieldrin, imidacloprid and profenofos. Exceedance of MRLs suggests a risk for the consumers and limits the opportunities of exportation. In order to define estimated daily intake, dietary surveys were conducted on 126 gardeners using a 24hours recall method. Single pesticide and cumulative exposure risks were assessed for children and adults. Risk was identified for: chlorpyrifos and lambda-cyhalothrin in acute and chronic exposure scenarios. Hazardous chronic exposure to the endocrine disruptor and probable carcinogen dieldrin was also detected. In the studied population, cumulative dietary exposure presented a risk (acute and chronic) for children and adults in respectively >17% and 4% of the cases when considering the worst case scenarios. Processing factor largely influenced the risk of occurrence suggesting that simple washing of vegetables with water considerably reduced the risk of hazardous exposure. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Fluorescence polarization immunoassay using IgY antibodies for detection of valnemulin in swine tissue.

    PubMed

    Zhang, Huiyan; Mi, Tiejun; Khan, Oleg Yu; Sheng, Yajie; Eremin, Sergei A; Beier, Ross C; Zhang, Suxia; Shen, Jianzhong; Wang, Zhanhui

    2015-10-01

    Immunoglobulin Y (IgY) is derived from egg yolk and has been identified as a cheap and high-yield immunoreagent. The application of IgY in immunoassays for the detection of chemical contaminants in food samples has rarely been reported. In this work, we describe a rapid and sensitive fluorescence polarization immunoassay (FPIA) for valnemulin (VAL) using IgY which was produced using a previously prepared immunogen. Three fluorophore-labeled VAL tracers were synthesized and the sensitivity of the best tracer (VAL-DTAF) in the optimized FPIA with antibody IgY100 demonstrated an IC50 value of 12 ng mL(-1) in buffer. After evaluation of several extraction procedures, acidified acetonitrile was selected to extract VAL from swine tissue. The recoveries of VAL in spiked swine tissue at three levels (50, 100, and 200 μg kg(-1)) were higher than 79% with coefficients of variation (CVs) lower than 12%. The limit of detection (LOD) of the FPIA in swine tissue was 26 μg kg(-1) and was lower than the maximum residue limit (MRL) of VAL set by the European Union. The study showed that IgY could be a good substitute for IgG when developing a high-throughput assay for chemical residues.

  9. A novel multiplexed fluorescence polarisation immunoassay based on a recombinant bi-specific single-chain diabody for simultaneous detection of fluoroquinolones and sulfonamides in milk.

    PubMed

    Chen, Min; Wen, Kai; Tao, Xiaoqi; Ding, Shuangyang; Xie, Jie; Yu, Xuezhi; Li, Jiancheng; Xia, Xi; Wang, Yang; Xie, Sanlei; Jiang, Haiyang

    2014-01-01

    Major research efforts are focusing on the development of simultaneous multiplexed immunoassays. In this study, a novel dual-binding fluorescence polarisation immunoassay (DB-FPIA) using a broad-specificity bi-specific single-chain diabody (scDb) and two fluorescent-labelled tracers (sulfamethoxypyridazine-fluorescein isothiocyanate (SMP-FITC) and sarafloxacin-Texas Red (SAR-TR)) with different excitation and emission wavelengths was developed for simultaneous and high-throughput detection of 19 fluoroquinolones (FQs) and 13 sulfonamides (SAs) at the maximum residue limits in milk samples. Recoveries for spiked milk samples were from 76.4% to 128.4%, with a relative standard deviation lower than 13.9%. The developed DB-FPIA was then applied to field samples, followed by confirmation by LC-MS/MS. All three instances in which FQs and SAs were present at concentrations near or above the assay limit of detection were identified as positive by the developed DB-FPIA, demonstrating that the method is suitable for rapid screening of FQs and SAs contamination. The novel methodology combines the advantage of the FPIA and the broad sensitivity of scDb and shows great promise for fast multi-analyte screening of low-molecular weight chemical residues in food samples.

  10. Pressurized liquid extraction combined with capillary electrophoresis-mass spectrometry as an improved methodology for the determination of sulfonamide residues in meat.

    PubMed

    Font, Guillermina; Juan-García, Ana; Picó, Yolanda

    2007-08-03

    A new analytical method, based on capillary electrophoresis and tandem mass spectrometry (CE-MS2), is proposed and validated for the identification and simultaneous quantification of 12 sulfonamides (SAs) in pork meat. The studied SAs include sulfathiazole, sulfadiazine, sulfamethoxypyridazine, sulfaguanidine, sulfanilamide, sulfadimethoxyne, sulfapyridine, sulfachloropyridazine, sulfisoxazole, sulfasalazine, sulfabenzamide and sulfadimidine. Different parameters (i.e. separation buffer, sheath liquid, electrospray conditions) were optimized to obtain an adequate CE separation and high MS sensitivity. MS2 experiments using an ion trap as analyzer, operating in the selected reaction monitoring (SRM) mode, were carried out to achieve the required number of identification points according to the 2002/657/EC European Decision. For the quantification in pork tissue samples, a pressurized liquid extraction (PLE) procedure, using hot water as extractant followed by an Oasis HLB cleanup, was developed. Linearity (r between 0.996 and 0.997), precision (RSD<14 %) and recoveries (from 76 to 98%) were satisfactory. The limits of detection and quantification (below 12.5 and 46.5 microg kg(-1), respectively) were in all cases lower than the maximum residue limits (MRLs), indicating the potential of CE-MS2 for the analysis of SAs, in the food quality and safety control areas.

  11. Identification of inorganic improvised explosive devices by analysis of postblast residues using portable capillary electrophoresis instrumentation and indirect photometric detection with a light-emitting diode.

    PubMed

    Hutchinson, Joseph P; Evenhuis, Christopher J; Johns, Cameron; Kazarian, Artaches A; Breadmore, Michael C; Macka, Miroslav; Hilder, Emily F; Guijt, Rosanne M; Dicinoski, Greg W; Haddad, Paul R

    2007-09-15

    A commercial portable capillary electrophoresis (CE) instrument has been used to separate inorganic anions and cations found in postblast residues from improvised explosive devices (IEDs) of the type used frequently in terrorism attacks. The purpose of this analysis was to identify the type of explosive used. The CE instrument was modified for use with an in-house miniaturized light-emitting diode (LED) detector to enable sensitive indirect photometric detection to be employed for the detection of 15 anions (acetate, benzoate, carbonate, chlorate, chloride, chlorite, cyanate, fluoride, nitrate, nitrite, perchlorate, phosphate, sulfate, thiocyanate, thiosulfate) and 12 cations (ammonium, monomethylammonium, ethylammonium, potassium, sodium, barium, strontium, magnesium, manganese, calcium, zinc, lead) as the target analytes. These ions are known to be present in postblast residues from inorganic IEDs constructed from ammonium nitrate/fuel oil mixtures, black powder, and chlorate/perchlorate/sugar mixtures. For the analysis of cations, a blue LED (470 nm) was used in conjunction with the highly absorbing cationic dye, chrysoidine (absorption maximum at 453 nm). A nonaqueous background electrolyte comprising 10 mM chrysoidine in methanol was found to give greatly improved baseline stability in comparison to aqueous electrolytes due to the increased solubility of chrysoidine and its decreased adsorption onto the capillary wall. Glacial acetic acid (0.7% v/v) was added to ensure chrysoidine was protonated and to enhance separation selectivity by means of complexation with transition metal ions. The 12 target cations were separated in less than 9.5 min with detection limits of 0.11-2.30 mg/L (calculated at a signal-to-noise ratio of 3). The anions separation system utilized a UV LED (370 nm) in conjunction with an aqueous chromate electrolyte (absorption maximum at 371 nm) consisting of 10 mM chromium(VI) oxide and 10 mM sodium chromate, buffered with 40 mM tris(hydroxymethyl)aminomethane at pH 8.05. All 15 target anions were baseline separated in less than 9 min with limits of detection ranging from 0.24 to 1.15 mg/L (calculated at a signal-to-noise ratio of 3). Use of the portable instrumentation in the field was demonstrated by analyzing postblast residues in a mobile laboratory immediately after detonation of the explosive devices. Profiling the ionic composition of the inorganic IEDs allowed identification of the chemicals used in their construction.

  12. Evaluation of pesticide residues of organochlorine in vegetables and fruits in Qatar: statistical analysis.

    PubMed

    Al-Shamary, Noora M; Al-Ghouti, Mohammad A; Al-Shaikh, Ismail; Al-Meer, Saeed H; Ahmad, Talaat A

    2016-03-01

    The study aimed to examine the residues of organochlorines pesticides (OCPs) in vegetables and fruits in Qatar. A total of 127 samples was studied. Ninety percent of the imported samples recorded residues above the maximum residue levels (MRLs). The most frequently detected OCP in the samples was heptachlor (found in 75 samples). In the comparisons between the washed and unwashed samples, no significant differences were observed (P > 0.05). However, the effect of washing process with tap water depended on the type of vegetables and fruits.

  13. Capillary Trapping of CO2 in Oil Reservoirs: Observations in a Mixed-Wet Carbonate Rock.

    PubMed

    Al-Menhali, Ali S; Krevor, Samuel

    2016-03-01

    Early deployment of carbon dioxide storage is likely to focus on injection into mature oil reservoirs, most of which occur in carbonate rock units. Observations and modeling have shown how capillary trapping leads to the immobilization of CO2 in saline aquifers, enhancing the security and capacity of storage. There are, however, no observations of trapping in rocks with a mixed-wet-state characteristic of hydrocarbon-bearing carbonate reservoirs. Here, we found that residual trapping of supercritical CO2 in a limestone altered to a mixed-wet state with oil was significantly less than trapping in the unaltered rock. In unaltered samples, the trapping of CO2 and N2 were indistinguishable, with a maximum residual saturation of 24%. After the alteration of the wetting state, the trapping of N2 was reduced, with a maximum residual saturation of 19%. The trapping of CO2 was reduced even further, with a maximum residual saturation of 15%. Best-fit Land-model constants shifted from C = 1.73 in the water-wet rock to C = 2.82 for N2 and C = 4.11 for the CO2 in the mixed-wet rock. The results indicate that plume migration will be less constrained by capillary trapping for CO2 storage projects using oil fields compared with those for saline aquifers.

  14. Impact of downward-mixing ozone on surface ozone accumulation in southern Taiwan.

    PubMed

    Lin, Ching-Ho

    2008-04-01

    The ozone that initially presents in the previous day's afternoon mixing layer can remain in the nighttime atmosphere and then be carried over to the next morning. Finally, this ozone can be brought to the ground by downward mixing as mixing depth increases during the daytime, thereby increasing surface ozone concentrations. Variation of ozone concentration during each of these periods is investigated in this work. First, ozone concentrations existing in the daily early morning atmosphere at the altitude range of the daily maximum mixing depth (residual ozone concentrations) were measured using tethered ozonesondes on 52 experimental days during 2004-2005 in southern Taiwan. Daily downward-mixing ozone concentrations were calculated by a box model coupling the measured daily residual ozone concentrations and daily mixing depth variations. The ozone concentrations upwind in the previous day's afternoon mixing layer were estimated by the combination of back air trajectory analysis and known previous day's surface ozone distributions. Additionally, the relationship between daily downward-mixing ozone concentration and daily photochemically produced ozone concentration was examined. The latter was calculated by removing the former from daily surface maximum ozone concentration. The measured daily residual ozone concentrations distributed at 12-74 parts per billion (ppb) with an average of 42 +/- 17 ppb are well correlated with the previous upwind ozone concentration (R2 = 0.54-0.65). Approximately 60% of the previous upwind ozone was estimated to be carried over to the next morning and became the observed residual ozone. The daily downward-mixing ozone contributes 48 +/- 18% of the daily surface maximum ozone concentration, indicating that the downward-mixing ozone is as important as daily photochemically produced ozone to daily surface maximum ozone accumulation. The daily downward-mixing ozone is poorly correlated with the daily photochemically produced ozone and contributes significantly to the daily variation of surface maximum ozone concentrations (R2 = 0.19). However, the contribution of downward-mixing ozone to daily ozone variation is not included in most existing statistical models developed for predicting daily ozone variation. Finally, daily surface maximum ozone concentration is positively correlated with daily afternoon mixing depth, attributable to the downward-mixing ozone.

  15. Multidetection of antibiotics in liver tissue by ultra-high-pressure-liquid-chromatography-tandem mass spectrometry.

    PubMed

    Freitas, Andreia; Barbosa, Jorge; Ramos, Fernando

    2015-01-22

    A multiresidue quantitative screening method covering 39 antibiotics from 7 different families by ultra-high-pressure-liquid-chromatography-tandem mass spectrometry (UHPLC-MS/MS) is described. Sulfonamides, trimethoprim, tetracyclines, macrolides, quinolones, penicillins and chloramphenicol are simultaneously detected in liver tissue. A simple sample treatment method consisting of extraction with a mixture of acetonitrile and ethylenediaminetetraacetic acid (EDTA) followed by solid-phase extraction (SPE) with a hydrophilic-lipophilic balanced (HLB) cartridge was developed. The methodology was validated, in accordance with Decision 2002/657/EC, by evaluating the following required parameters: decision limit (CCα), detection capability (CCβ), specificity, repeatability and reproducibility. The precision, in terms of the relative standard deviation, was under 22% for all of the compounds, and the recoveries were between 80% and 110%. The CCα and CCβ were determined according to the maximum residue limit (MRL) or the minimum required performance limit (MRPL), when established. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Pretreatment of bamboo residues with Coriolus versicolor for enzymatic hydrolysis.

    PubMed

    Zhang, Xiaoyu; Xu, Chunyan; Wang, Hongxun

    2007-08-01

    Pretreatment by a white-rot fungus Coriolus versicolor B1 under different conditions and saccharification of bamboo were investigated. The saccharification rate was significantly enhanced and a maximum saccharification rate of 37.0% was achieved after pretreatment. Reducing sugars yield was 223.2 mg/g of bamboo residues, which was 2.34 times that of the raw material. It was feasible to treat bamboo residues with B1 for the saccharification of bamboo.

  17. Nanohardness and Residual Stress in TiN Coatings.

    PubMed

    Hernández, Luis Carlos; Ponce, Luis; Fundora, Abel; López, Enrique; Pérez, Eduardo

    2011-05-17

    TiN films were prepared by the Cathodic arc evaporation deposition method under different negative substrate bias. AFM image analyses show that the growth mode of biased coatings changes from 3D island to lateral when the negative bias potential is increased. Nanohardness of the thin films was measured by nanoindentation, and residual stress was determined using Grazing incidence X ray diffraction. The maximum value of residual stress is reached at -100 V substrate bias coinciding with the biggest values of adhesion and nanohardness. Nanoindentation measurement proves that the force-depth curve shifts due to residual stress. The experimental results demonstrate that nanohardness is seriously affected by the residual stress.

  18. Choosing Models for Health Care Cost Analyses: Issues of Nonlinearity and Endogeneity

    PubMed Central

    Garrido, Melissa M; Deb, Partha; Burgess, James F; Penrod, Joan D

    2012-01-01

    Objective To compare methods of analyzing endogenous treatment effect models for nonlinear outcomes and illustrate the impact of model specification on estimates of treatment effects such as health care costs. Data Sources Secondary data on cost and utilization for inpatients hospitalized in five Veterans Affairs acute care facilities in 2005–2006. Study Design We compare results from analyses with full information maximum simulated likelihood (FIMSL); control function (CF) approaches employing different types and functional forms for the residuals, including the special case of two-stage residual inclusion; and two-stage least squares (2SLS). As an example, we examine the effect of an inpatient palliative care (PC) consultation on direct costs of care per day. Data Collection/Extraction Methods We analyzed data for 3,389 inpatients with one or more life-limiting diseases. Principal Findings The distribution of average treatment effects on the treated and local average treatment effects of a PC consultation depended on model specification. CF and FIMSL estimates were more similar to each other than to 2SLS estimates. CF estimates were sensitive to choice and functional form of residual. Conclusions When modeling cost or other nonlinear data with endogeneity, one should be aware of the impact of model specification and treatment effect choice on results. PMID:22524165

  19. Distribution of chlorpyrifos in rice paddy environment and its potential dietary risk.

    PubMed

    Fu, Yan; Liu, Feifei; Zhao, Chenglin; Zhao, Ying; Liu, Yihua; Zhu, Guonian

    2015-09-01

    Chlorpyrifos is one of the most extensively used insecticides in China. The distribution and residues of chlorpyrifos in a paddy environment were characterized under field and laboratory conditions. The half-lives of chlorpyrifos in the two conditions were 0.9-3.8days (field) and 2.8-10.3days (laboratory), respectively. The initial distribution of chlorpyrifos followed the increasing order of water

  20. Comparison of a new air-assisted sprayer and two conventional sprayers in terms of deposition, loss to the soil and residue of azoxystrobin and tebuconazole applied to sunlit greenhouse tomato and field cucumber.

    PubMed

    Li, Yanjie; Li, Yifan; Pan, Xiang; Li, Qing X; Chen, Ronghua; Li, Xuesheng; Pan, Canping; Song, Jianli

    2018-02-01

    Plant protection products (PPPs) are applied in China and many other developing countries with knapsack sprayers at high volumes with coarse spray quality, resulting in a high percentage of pesticide losses. In this study, a new air-assisted electric knapsack sprayer and two conventional knapsack sprayers were evaluated in terms of pesticide deposition, residues and loss into the soil. Artificial targets fixed to the upper side and underside of the leaf surface in six zones (at two depths and three heights) were used to collect the deposition, which were analyzed by liquid chromatography triple-quadrupole mass spectrometry. The air-assisted electric knapsack sprayer produced more deposition and better penetrability and uniformity than the two traditional spraying methods. In particular, the air-assisted electric knapsack sprayer reduced pesticide losses to the soil by roughly 37% to 75% and deposited 1.18 and 1.24 times more pesticide than the manual air-pressure and battery-powered knapsack sprayers, respectively. The residues of azoxystrobin and tebuconazole in tomato and cucumber were below the maximum residue limits (MRLs). In general, use of the the air-assisted electric knapsack sprayer in tomato and cucumber crops could improve the effectiveness of PPPs, reduce the risk of contamination and protect food safety. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  1. Assessment of single-shell tank residual-liquid issues at Hanford Site, Washington

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Murthy, K.S.; Stout, L.A.; Napier, B.A.

    1983-06-01

    This report provides an assessment of the overall effectiveness and implications of jet pumping the interstitial liquids (IL) from single-shell tanks at Hanford. The jet-pumping program, currently in progress at Hanford, involves the planned removal of IL contained in 89 of the 149 single-shell tanks and its transfer to double-shell tanks after volume reduction by evaporation. The purpose of this report is to estimate the public and worker doses associated with (1) terminating pumping immediately, (2) pumping to a 100,000-gal limit per tank, (3) pumping to a 50,000-gal limit per tank, and (4) pumping to the maximum practical liquid removalmore » level of 30,000 gal. Assessment of the cost-effectiveness of these various levels of pumping in minimizing any undue health and safety risks to the public or worker is also presented.« less

  2. A study of fiber volume fraction effects in notched unidirectional SCS-6/Ti-15V-3Cr-3Al-3Sn composite. Ph.D. Thesis Final Report

    NASA Technical Reports Server (NTRS)

    Covey, Steven J.

    1993-01-01

    Notched unidirectional SCS-6/Ti-15-3 composite of three different fiber volume fractions (vf = 0.15, 0.37, and 0.41) was investigated for various room temperature microstructural and material properties including: fatigue crack initiation, fatigue crack growth, and fracture toughness. While the matrix hardness is similar for all fiber volume fractions, the fiber/matrix interfacial shear strength and matrix residual stress increases with fiber volume fraction. The composite fatigue crack initiation stress is shown to be matrix controlled and occurs when the net maximum matrix stress approaches the endurance limit stress of the matrix. A model is presented which includes residual stresses and presents the composite initiation stress as a function of fiber volume fraction. This model predicts a maximum composite initiation stress at vf approximately 0.15 which agrees with the experimental data. The applied composite stress levels were increased as necessary for continued crack growth. The applied Delta(K) values at crack arrest increase with fiber volume fraction by an amount better approximated using an energy based formulation rather than when scaled linear with modulus. After crack arrest, the crack growth rate exponents for vf37 and vf41 were much lower and toughness much higher, when compared to the unreinforced matrix, because of the bridged region which parades with the propagating fatigue crack. However, the vf15 material exhibited a higher crack growth rate exponent and lower toughness than the unreinforced matrix because once the bridged fibers nearest the crack mouth broke, the stress redistribution broke all bridged fibers, leaving an unbridged crack. Degraded, unbridged behavior is modeled using the residual stress state in the matrix ahead of the crack tip. Plastic zone sizes were directly measured using a metallographic technique and allow prediction of an effective matrix stress intensity which agrees with the fiber pressure model if residual stresses are considered. The sophisticated macro/micro finite element models of the 0.15 and 0.37 fiber volume fractions presented show good agreement with experimental data and the fiber pressure model when an estimated effective fiber/matrix debond length is used.

  3. Oxytetracycline and penicillin-G residues in cattle slaughtered in south-western Nigeria: implications for livestock disease management and public health.

    PubMed

    Adesokan, Hezekiah K; Agada, Charity A; Adetunji, Victoria O; Akanbi, Ibikunle M

    2013-01-01

    After the discovery of indiscriminate antibiotic use in ready-for-slaughter cattle in south-western Nigeria, 90 tissue samples from randomly selected slaughtered cattle were evaluated for oxytetracycline and penicillin-G residues using high performance liquid chromatography and the data analysed by one-way Analysis of variance (ANOVA). The findings revealed residues of oxytetracycline (kidney: 9.47 µ/kg ± 3.24 µ/kg; liver: 12.73 µ/kg ± 4.39 µ/kg; muscle: 16.17 µ/kg ± 5.52 µ/kg) and penicillin-G (kidney: 6.27 µ/kg ± 2.46 µ/kg; liver: 8.5 µ/kg ± 2.80 µ/kg; muscle: 11.67 µ/kg ± 2.94 µ/kg) in all tissues screened. Significantly high levels (oxytetracycline: F = 16.77; penicillin-G: F = 29.38) were, however, found in muscles, followed by liver and then kidney – findings confirming recent antibiotic administration to the animals before slaughter. The dietary intakes through the tissues screened were 0.024% (oxytetracycline) and 0.017% (penicillin-G) of the acceptable daily intake (ADI). Although the concentrations in the tissues screened were below the maximum residue limits despite recent administration of these antibiotics before slaughter, the lower concentrations are suggestive of the probable low dosages often administered by those involved in indiscriminate use of antibiotics. This therefore raises serious concerns for the livestock industry as well as human health, given the resultant emergence and spread of resistant strains of bacterial pathogens that could ensue from prolonged use of low dosages of antibiotics. Additionally, the lower concentrations of the daily intakes notwithstanding, the plausible exposure to these antibiotics from other food sources is a cause for concern. Since antimicrobial misuse and its consequent effects are not just a problem limited to Nigeria but also a concern in sub-Saharan Africa, the need for national and international stakeholder intervention is emphasised.

  4. Fate of ivermectin residues in ewes' milk and derived products.

    PubMed

    Cerkvenik, Vesna; Perko, Bogdan; Rogelj, Irena; Doganoc, Darinka Z; Skubic, Valentin; Beek, Wim M J; Keukens, Henk J

    2004-02-01

    The fate of ivermectin (IVM) residues was studied throughout the processing of daily bulk milk from 30 ewes (taken up to 33 d following subcutaneous administration of 0.2 mg IVM/kg b.w.) in the following milk products: yoghurt made from raw and pasteurized milk; cheese after pressing; 30- and 60-day ripened cheese; and whey, secondary whey and whey proteins obtained after cheese-making (albumin cheese). The concentration of the H2B1a component of IVM was analysed in these dairy products using an HPLC method with fluorescence detection. The mean recovery of the method was, depending on the matrix, between 87 and 100%. Limits of detection in the order of only 0.1 microg H2B1a/kg of product were achieved. Maximum concentrations of IVM were detected mostly at 2 d after drug administration to the ewes. The highest concentration of IVM was found on day 2 in 60-day ripened cheese (96 microg H2B1a/kg cheese). Secondary whey was the matrix with the lowest concentration of IVM (<0.6 microg H2B1a/ kg). Residue levels fell below the limits of detection between day 5 (for secondary whey) and day 25 (for all cheese samples). In the matrices investigated, linear correlations between daily concentrations of IVM, milk fat and solid content were evident. During yoghurt production, fermentation and thermal stability of IVM was observed. During cheese production, approximately 35% of the IVM, present in the raw (bulk) milk samples, was lost. From the results it was concluded that the processing of ewes' milk did not eliminate the drug residues under investigation. The consequences of IVM in the human diet were discussed. Milk from treated animals should be excluded from production of fat products like cheese for longer after treatment with IVM than for lower fat products.

  5. Acaricide Residues in Laying Hens Naturally Infested by Red Mite Dermanyssus gallinae

    PubMed Central

    Marangi, Marianna; Morelli, Vincenzo; Pati, Sandra; Camarda, Antonio; Cafiero, Maria Assunta; Giangaspero, Annunziata

    2012-01-01

    In the poultry industry, control of the red mite D. gallinae primarily relies worldwide on acaricides registered for use in agriculture or for livestock, and those most widely used are carbamates, followed by amidines, pyrethroids and organophosphates. Due to the repeated use of acaricides - sometimes in high concentrations - to control infestation, red mites may become resistant, and acaricides may accumulate in chicken organs and tissues, and also in eggs. To highlight some situations of misuse/abuse of chemicals and of risk to human health, we investigated laying hens, destined to the slaughterhouse, for the presence of acaricide residues in their organs and tissues. We used 45 hens from which we collected a total of 225 samples from the following tissues and organs: skin, fat, liver, muscle, hearth, and kidney. In these samples we analyzed the residual contents of carbaryl and permethrin by LC-MS/MS. Ninety-one (40.4%) samples were positive to carbaryl and four samples (1.7%) were positive to permethrin. Concentrations of carbaryl exceeding the detection limit (0.005 ppm) were registered in the skin and fat of birds from two farms (p<0.01), although these concentrations remained below the maximum residue limit (MRLs) (0.05 ppm) (p<0.01). All organs/tissues of hens from a third farm were significantly more contaminated, with skin and muscle samples exceeding the MRL (0.05 ppm) (p<0.01) of carbaryl in force before its use was banned. Out of 45 chickens tested, 37 (82.2%) were found to be contaminated by carbaryl, and 4 (8.8%) by permethrin. The present study is the first report on the presence of pesticides banned by the EU (carbaryl) or not licensed for use (permethrin) in the organs and tissues of laying hens, which have been treated against red mites, and then slaughtered for human consumption at the end of their life cycle. PMID:22363736

  6. Acaricide residues in laying hens naturally infested by red mite Dermanyssus gallinae.

    PubMed

    Marangi, Marianna; Morelli, Vincenzo; Pati, Sandra; Camarda, Antonio; Cafiero, Maria Assunta; Giangaspero, Annunziata

    2012-01-01

    In the poultry industry, control of the red mite D. gallinae primarily relies worldwide on acaricides registered for use in agriculture or for livestock, and those most widely used are carbamates, followed by amidines, pyrethroids and organophosphates. Due to the repeated use of acaricides--sometimes in high concentrations--to control infestation, red mites may become resistant, and acaricides may accumulate in chicken organs and tissues, and also in eggs. To highlight some situations of misuse/abuse of chemicals and of risk to human health, we investigated laying hens, destined to the slaughterhouse, for the presence of acaricide residues in their organs and tissues. We used 45 hens from which we collected a total of 225 samples from the following tissues and organs: skin, fat, liver, muscle, hearth, and kidney. In these samples we analyzed the residual contents of carbaryl and permethrin by LC-MS/MS.Ninety-one (40.4%) samples were positive to carbaryl and four samples (1.7%) were positive to permethrin. Concentrations of carbaryl exceeding the detection limit (0.005 ppm) were registered in the skin and fat of birds from two farms (p<0.01), although these concentrations remained below the maximum residue limit (MRLs) (0.05 ppm) (p<0.01). All organs/tissues of hens from a third farm were significantly more contaminated, with skin and muscle samples exceeding the MRL (0.05 ppm) (p<0.01) of carbaryl in force before its use was banned. Out of 45 chickens tested, 37 (82.2%) were found to be contaminated by carbaryl, and 4 (8.8%) by permethrin. The present study is the first report on the presence of pesticides banned by the EU (carbaryl) or not licensed for use (permethrin) in the organs and tissues of laying hens, which have been treated against red mites, and then slaughtered for human consumption at the end of their life cycle.

  7. Crop residue is key for sustaining maximum food production and for conservation of our biosphere

    USDA-ARS?s Scientific Manuscript database

    Crop residue is key in our efforts to move towards agricultural sustainability. This paper provides a quick overview of some selected references and looks at some of the newest advances related to cover crops. Several authors have described in detail the benefits derived from improving soil quality ...

  8. Three-dimensional local residual stress and orientation gradients near graphite nodules in ductile cast iron [3D local residual stress and orientation gradients near graphite nodules in ductile cast iron

    DOE PAGES

    Zhang, Y. B.; Andriollo, T.; Faester, S.; ...

    2016-09-14

    A synchrotron technique, differential aperture X-ray microscopy (DAXM), has been applied to characterize the microstructure and analyze the local mesoscale residual elastic strain fields around graphite nodules embedded in ferrite matrix grains in ductile cast iron. Compressive residual elastic strains are measured with a maximum strain of ~6.5–8 × 10 –4 near the graphite nodules extending into the matrix about 20 μm, where the elastic strain is near zero. The experimental data are compared with a strain gradient calculated by a finite element model, and good accord has been found but with a significant overprediction of the maximum strain. Thismore » is discussed in terms of stress relaxation during cooling or during storage by plastic deformation of the nodule, the matrix or both. Furthermore, relaxation by plastic deformation of the ferrite is demonstrated by the formation of low energy dislocation cell structure also quantified by the DAXM technique.« less

  9. Effects of Storage of CPD-ADSOL Red Cells at 4C for as Long as 49 Days, Biochemical Modification, Freeze-Preservation, and Post-Wash Storage at 4C for 24 Hours

    DTIC Science & Technology

    1992-05-27

    DPG, P50 levels , and the level of residual hemolysis were satisfactory. Our data show that 42-days is the maximum period that red blood cells can...survival value of only 61%, but ATP, DPG, P50 levels and the level of residual hemolysis were satisfactory. Our data show that 42-days is the maximum...collected red blood cells are stored at 4C for less than 2 weeks, the rejuventation process increases the red cell 2,3 DPG level to 250% of normal and the

  10. Topographic enhancement of tidal motion in the western Barents Sea

    NASA Technical Reports Server (NTRS)

    Kowalik, Z.; Proshutinsky, A. YU.

    1995-01-01

    A high-resolution numerical lattice is used to study a topographically trapped motion around islands and shallow banks of the western Barents Sea caused both by the semidiurnal and diurnal tidal waves. Observations and model computations in the vicinity of Bear Island show well-developed trapped motion with distinctive tidal oscillatory motion. Numerical investigations demonstrate that one source of the trapped motion is tidal current rectification over shallow topgraphy. Tidal motion supports residual currents of the order of 8 cm/s around Bear Island and shallow Spitsbergenbanken. The structures of enhanced tidal currents for the semidiurnal components are generated in the shallow areas due to topographic amplification. In the diurnal band of oscillations the maximum current is associated with the shelf wave occurrence. Residual currents due to diurnal tides occur at both the shallow areas and the shelf slope in regions of maximum topographic gradients. Surface manifestation of the diurnal current enhancement is the local maximum of tidal amplitude at the shelf break of the order of 5 to 10 cm. Tidal current enhancement and tidally generated residual currents in the Bear Island and Spitsbergenabanken regions cause an increased generation of ice leads, ridges and, trapped motion of the ice floes.

  11. Evaluation of a microbiological indicator test for antibiotic detection in ewe and goat milk.

    PubMed

    Comunian, R; Paba, A; Dupré, I; Daga, E S; Scintu, M F

    2010-12-01

    Antibiotics are widely used for therapeutic and prophylactic purposes in dairy animals. The presence of residual antibiotics in milk could cause potentially serious problems in human health and have technological implication in the manufacturing of dairy products. The aim of this study was to evaluate Delvotest Accelerator (DSM Food Specialties, Delft, the Netherlands), a new system for a fully automated microbial test to detect antibiotic residues in ewe and goat milk. Forty-three samples of raw, whole, refrigerated bulk-tank milk samples (22 of ewe milk and 21 of goat milk) were analyzed during the whole lactation period. Four concentrations of 4 antibiotics were diluted in milk: penicillin G at 1, 2, 3, and 4 μg/L; sulfadiazine at 25, 50, 100, and 200 μg/L; tetracycline at 50, 100, 200, and 400 μg/L; and gentamicin at 25, 50, 100, and 200 μg/L. The detection limit of the Delvotest Accelerator was calculated as the range of antibiotic concentrations within which 95% of positive result lie. The range of detection limit of penicillin G and sulfadiazine was easily detected by Delvotest Accelerator at or below the European Union maximum residue limits, both for ewe and goat milk samples. In contrast, the system showed a lower ability to detect tetracycline and gentamicin both for ewe and goat milk samples. Very low percentages of false-positive outcomes were obtained. Lactation phase did not seem to be a crucial factor affecting the ability of the Delvotest Accelerator to detect spiked milk samples. A higher detection ability was observed for goat milk samples compared with ewe milk samples. A negative correlation between the percentage of positive milk samples detected and milk fat, protein, and lactose contents was observed for gentamicin only. Copyright © 2010 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  12. Evaluation of the Charm maximum residue limit β-lactam and tetracycline test for the detection of antibiotics in ewe and goat milk.

    PubMed

    Beltrán, M C; Romero, T; Althaus, R L; Molina, M P

    2013-05-01

    The Charm maximum residue limit β-lactam and tetracycline test (Charm MRL BLTET; Charm Sciences Inc., Lawrence, MA) is an immunoreceptor assay utilizing Rapid One-Step Assay lateral flow technology that detects β-lactam or tetracycline drugs in raw commingled cow milk at or below European Union maximum residue levels (EU-MRL). The Charm MRL BLTET test procedure was recently modified (dilution in buffer and longer incubation) by the manufacturers to be used with raw ewe and goat milk. To assess the Charm MRL BLTET test for the detection of β-lactams and tetracyclines in milk of small ruminants, an evaluation study was performed at Instituto de Ciencia y Tecnologia Animal of Universitat Politècnica de València (Spain). The test specificity and detection capability (CCβ) were studied following Commission Decision 2002/657/EC. Specificity results obtained in this study were optimal for individual milk free of antimicrobials from ewes (99.2% for β-lactams and 100% for tetracyclines) and goats (97.9% for β-lactams and 100% for tetracyclines) along the entire lactation period regardless of whether the results were visually or instrumentally interpreted. Moreover, no positive results were obtained when a relatively high concentration of different substances belonging to antimicrobial families other than β-lactams and tetracyclines were present in ewe and goat milk. For both types of milk, the CCβ calculated was lower or equal to EU-MRL for amoxicillin (4 µg/kg), ampicillin (4 µg/kg), benzylpenicillin (≤ 2 µg/kg), dicloxacillin (30 µg/kg), oxacillin (30 µg/kg), cefacetrile (≤ 63 µg/kg), cefalonium (≤ 10 µg/kg), cefapirin (≤ 30 µg/kg), desacetylcefapirin (≤ 30 µg/kg), cefazolin (≤ 25 µg/kg), cefoperazone (≤ 25 µg/kg), cefquinome (20 µg/kg), ceftiofur (≤ 50 µg/kg), desfuroylceftiofur (≤ 50µg/kg), and cephalexin (≤ 50 µg/kg). However, this test could neither detect cloxacillin nor nafcillin at or below EU-MRL (CCβ >30 µg/kg). The CCβ for tetracyclines was also lower than EU-MRL for chlortetracycline (ewe milk: ≤ 50 µg/kg; goat milk: 75 µg/kg), oxytetracycline (≤ 50 µg/kg), and tetracycline (≤ 50 µg/kg). Regarding the 4-epimers of these tetracyclines only 4-epioxytetracycline was detected by the Charm MRL BLTET test below EU-MRL (ewe milk: 75 µg/kg; goat milk: ≤ 50 µg/kg). Acidiol had no effect on the performance of the test. The Charm MRL BLTET test could be used routinely with adapted test procedure for the fast screening of ewe and goat milk. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  13. Concentration of Mercury in Cockles (Anadara granosa and A. antiquata) Harvested from Estuaries of Western Lombok, Indonesia, and Potential Risks to Human Health.

    PubMed

    Rahayu, Rachmawati Noviana; Irawan, Bambang; Soegianto, Agoes

    2016-01-01

    This study measured the levels of total mercury (tHg) in the whole tissues of cockles (Anadara granosa and A. antiquata) harvested from three estuaries of Western Lombok Island (WLI), Indonesia. This paper also evaluated the hazard level posed by the mercury in relation to the maximum residual limit for human consumption and to estimate the weekly intake and compare it with the provisional tolerable weekly intake (PTWI). The tHg concentrations in A. granosa ranged from 0.020 to 0.070 mg kg(-1), and those in A. antiquata were between 0.032 and 0.077 mg kg(-1) at all locations. All samples of cockles harvested from WLI contain tHg below the permissible limit for human consumption. The maximum weekly intakes for total mercury by coastal people range from 0.28 to 1.08 µg kg(-1) b.w., and they are below the recommended values of PTWI (5.6 µg kg(-1) b.w.). If it is assumed that 100% of the Hg in cockles is methyl mercury (MeHg), consumption of the indicated amounts at the measured values wouldn't exceed the MeHg PTWI (1.6 µg kg(-1) b.w.).

  14. Plant protection product residues in white grapes and wines of "Malvasia Istriana" produced in Istria.

    PubMed

    Baša Česnik, Helena; Velikonja Bolta, Špela; Bavčar, Dejan; Radeka, Sanja; Lisjak, Klemen

    2016-12-01

    Monitorting of plant protection product residues was performed in 12 grape and 66 wine samples of "Malvasia Istriana" variety, produced in Istria winegrowing region of Croatia and Slovenia. The samples were analysed for the presence of 169 different active compounds using two multiresidual analytical methods: gas chromatography coupled with mass spectrometry and liquid chromatography coupled with tandem mass spectrometry. Residues were found in 58.3% of all the inspected grape samples and in 28.8% of all the inspected wine samples. Beside that contents of residues in grapes were below 10% of maximum residue level values and they should not represent any risk for "Malvasia Istriana" grape or wine consumers.

  15. Comparison of artificial maturation of lignite in hydrous and nonhydrous conditions

    USGS Publications Warehouse

    Behar, F.; Lewan, M.D.; Lorant, F.; Vandenbroucke, M.

    2003-01-01

    The objectives of the study are to compare product compositions and yields generated from lignite artificially matured by open nonhydrous pyrolysis, closed nonhydrous pyrolysis, and hydrous pyrolysis. The pyrolysis products were fractionated into CO2, H2O, CH4, C2-C5, C8-C14, C14+ saturates, C14+ aromatics and NSOs (resins+asphaltenes). All three methods generated high and similar quantities of water during pyrolysis that ranged between 14.6 and 15.2 wt.% of the original lignite. As a result of this high water content generated by the lignite, the experiments with no added water are referred to as nonhydrous rather than anhydrous. Rock-Eval pyrolysis and elemental analyses were conducted on the recovered lignite after solvent extraction to determine their residual hydrocarbon generation potential and to plot their position in a van Krevelen diagram, respectively. Residual lignite from the closed nonhydrous and hydrous experiments showed relationships between vitrinite reflectance (%Ro) values and atomic H/C ratios that occurred within the fields observed for natural maturation of coal. Although no significant differences in the atomic H/C ratios were observed between closed nonhydrous and hydrous pyrolysis, the vitrinite reflectance values were on the average 0.2% Ro lower in the residual lignite from the nonhydrous experiments. The remaining hydrocarbon generation potential as determined by Rock-Eval pyrolysis of the residual lignite showed that the nonhydrous residuals had on the average 16 mg more hydrocarbon potential per gram of original lignite than the hydrous residuals. This suggests there is a better release of the pyrolysis products from the lignite network in the hydrous experiments once generation occurs. For gas generation, at maximum yields, open nonhydrous pyrolysis generates the most hydrocarbon gas (21.0 mg/g original lignite), which is 20% more than closed nonhydrous pyrolysis and 29% more than hydrous pyrolysis. Closed nonhydrous pyrolysis generates on the average 14% more gas than hydrous pyrolysis, but the proportionality of the generated hydrocarbon gases is essentially the same for both pyrolysis methods. At maximum yields, CO2 generation is greatest in hydrous pyrolysis (99.5 mg/g original lignite), with yields being 37 percent higher than closed nonhydrous pyrolysis and 26% higher than open nonhydrous pyrolysis. The maximum yields of C14+ products are highest and similar for open nonhydrous pyrolysis and hydrous pyrolysis (125.6 and 125.9 mg/g lignite, respectively), and are more than 70% higher than closed nonhydrous pyrolysis. This difference in the maximum yields of C14+ products can be explained by differences in the proportionality between either cracking reactions that result in liquid product and char formation or trapping of generated products within the coal network (cross-linking reactions). Maximum yields of C14+ aliphatics from hydrous experiments may not have been attained, but the maximums that were observed and their GC traces are similar for the three pyrolysis systems.

  16. Stochastic modelling of the monthly average maximum and minimum temperature patterns in India 1981-2015

    NASA Astrophysics Data System (ADS)

    Narasimha Murthy, K. V.; Saravana, R.; Vijaya Kumar, K.

    2018-04-01

    The paper investigates the stochastic modelling and forecasting of monthly average maximum and minimum temperature patterns through suitable seasonal auto regressive integrated moving average (SARIMA) model for the period 1981-2015 in India. The variations and distributions of monthly maximum and minimum temperatures are analyzed through Box plots and cumulative distribution functions. The time series plot indicates that the maximum temperature series contain sharp peaks in almost all the years, while it is not true for the minimum temperature series, so both the series are modelled separately. The possible SARIMA model has been chosen based on observing autocorrelation function (ACF), partial autocorrelation function (PACF), and inverse autocorrelation function (IACF) of the logarithmic transformed temperature series. The SARIMA (1, 0, 0) × (0, 1, 1)12 model is selected for monthly average maximum and minimum temperature series based on minimum Bayesian information criteria. The model parameters are obtained using maximum-likelihood method with the help of standard error of residuals. The adequacy of the selected model is determined using correlation diagnostic checking through ACF, PACF, IACF, and p values of Ljung-Box test statistic of residuals and using normal diagnostic checking through the kernel and normal density curves of histogram and Q-Q plot. Finally, the forecasting of monthly maximum and minimum temperature patterns of India for the next 3 years has been noticed with the help of selected model.

  17. Leaching of Clothianidin in Two Different Indian Soils: Effect of Organic Amendment.

    PubMed

    Singh, Ningthoujam Samarendra; Mukherjee, Irani; Das, Shaon Kumar; Varghese, E

    2018-04-01

    Clothianidin is a widely used insecticide under Indian subtropical condition. The objective of this study was to generate residue data which aims to understand leaching potential of clothianidin [(E)-1-(2-chloro-1,3-thiazol-5-ylmethyl)-3-methyl-2- nitroguanidine] through packed soil column. The maximum amount of clothianidin was recovered at 0-5 cm soil depth in both Manipur (67.15%) and Delhi soil (52.0%) under continuous flow condition. Manipur and Delhi soil concentrated maximum residue with or without farm yard manure (FYM) in 0-20 cm soil depth. The effect of varying the amount of water enhanced the distribution of residues in the first 0-5 cm layer. Among the tested soils, residue was detected in the leachate from Delhi soil (0.04 µg/mL). Clothianidin leaching was minimized in soil of Manipur compared to Delhi after incorporation of FYM. As the volume of water increased upto 160 mL, mobility increased and residues moved to lower depth. Clothianidin did not leach out of the 25 cm long soil columns even after percolating water equivalent to 415.42 mm rainfall. Clothianidin is mobile in soil system and mobility can be reduced by organic amendment application.

  18. Numerical Analysis of Residual Stress and Distortion Use Finite Element Method on Inner Bottom Construction of Geomarin IV Survey Ship with Welding Sequence Variations

    NASA Astrophysics Data System (ADS)

    Syahroni, N.; Hartono, A. B. W.; Murtedjo, M.

    2018-03-01

    In the ship fabrication industry, welding is the most critical stage. If the quality of welding on ship fabrication is not good, then it will affect the strength and overall appearance of the structure. One of the factors that affect the quality of welding is residual stress and distortion. In this research welding simulation is performed on the inner bottom construction of Geomarin IV Ship Survey using shell element and has variation to welding sequence. In this study, welding simulations produced peak temperatures at 2490 K at variation 4. While the lowest peak temperature was produced by variation 2 with a temperature of 2339 K. After welding simulation, it continued simulating residual stresses and distortion. The smallest maximum tensile residual stress found in the inner bottom construction is 375.23 MPa, and the maximum tensile pressure is -20.18 MPa. The residual stress is obtained from variation 3. The distortion occurring in the inner bottom construction for X=720 mm is 4.2 mm and for X=-720 mm, the distortion is 4.92 mm. The distortion is obtained from the variation 3. Near the welding area, distortion value reaches its minimum point. This is because the stiffeners in the form of frames serves as anchoring.

  19. A case study on toxicological aspects of the pest and disease control in the production of the high-quality raspberry (Rubus idaeus L.).

    PubMed

    Sadło, Stanisław; Szpyrka, Ewa; Piechowicz, Bartosz; Grodzicki, Przemysław

    2015-01-01

    The field studies on the residue levels of the fungicides and insecticides used in commercial raspberry (Rubus idaeus L.) plantation have been performed. Starting on the first day of harvesting (on June 19), 20 laboratory samples of fruit, 10 laboratory samples of leaves and 4 samples of soil were analyzed and the residue levels were compared to the Maximum Residue Limits (MRL) and Acceptable Daily Intakes (ADI). All analyses were carried out using extraction method and gas chromatography technique. Esfenwalerate (Sumi-alpha 050 EC) and beta-cyfluthrin (Bulldock 025 EC), the insecticides belonging to the group of synthetic pyrethroids, were not found in harvested ripe fruits, while cypermethrin residues (Cyperkill 25 EC) applied on May 24, 25 days later was still found on low levels in fruits (0.026 mg kg(-1)) and in leaves (2.58 mg kg(-1)). In turn, residues of chlorpyrifos (Dursban 480 EC), applied to the soil on May 15 against the cockchafers Melolontha melolontha and Otiorhynchus sp., were found at the level 0.004 mg kg(-1). The content of pesticides in ripe fruits depended mainly on the dose and on the time that has elapsed from the date of their application and were as follows: boscalid -0.950, pyrimethanil -0.917, pyraclostrobin -0.253 cypermethrin -0.026 and chlorpyrifos -0.004 mg kg(-1) while in leaves: boscalid -30.64, pyrimethanil -8.13, pyraclostrobin -15.82, cypermethrin -2.58 and chlorpyrifos -0.15 mg kg(-1). The highest average daily intake was in the case of boscalid, and in fruits and leaves reached the levels 0.205 and 6.63, in total 0.33% and 12.18% of ADI, respectively.

  20. Organophosphorus pesticide residues in vegetables from farms, markets, and a supermarket around Kwan Phayao Lake of Northern Thailand.

    PubMed

    Sapbamrer, Ratana; Hongsibsong, Surat

    2014-07-01

    This study investigated organophosphorus (OP) residues in vegetables from 27 farms, 106 markets, and 1 supermarket around Kwan Phayao Lake, Northern Thailand, between August and September 2013. Types of vegetables sampled were all vegetables cultivated or sold around the study site. The most common OP pesticides detected in farm samples were chlorpyrifos (50 %), malathion (31.8 %), monocrotophos (31.8 %), diazinon (13.6 %), omethoate (13.6 %), and dicrotophos (9.1 %). The most common OP pesticides detected in market samples were chlorpyrifos (33.9 %), diazinon (18.6 %), parathion-methyl (3.4 %), profenofos (3.4 %), primiphos-ethyl (3.4 %), and fenitrothion (1.7 %). The OP pesticides detected in supermarket samples were chlorpyrifos (33.3 %), and diazinon (66.7 %). Among the compounds detected, chlorpyrifos was detected in most of the vegetable samples from all sources. The highest chlorpyrifos level in farm samples were found in lemon balm (2.423 mg/kg) followed by Vietnamese coriander (0.835 mg/kg), and cowpea (0.027 mg/kg). The highest level in markets samples were found in garlic (7.785 mg/kg) followed by Chinese cabbage (2.864 mg/kg) and Vietnamese coriander (1.308 mg/kg). Residues from supermarket samples were found only in parsley (0.027 mg/kg). The findings showed that 16 samples (59.3 %) from farms and 14 samples (13.2 %) from markets contained OP residues at or above the maximum residue limits established by the European Union. It is concluded that awareness, safety education, and strict regulation of pesticide use are necessary.

  1. Strategies for the screening of antibiotic residues in eggs: comparison of the validation of the classical microbiological method with an immunobiosensor method.

    PubMed

    Gaudin, Valérie; Rault, Annie; Hedou, Celine; Soumet, Christophe; Verdon, Eric

    2017-09-01

    Efficient screening methods are needed to control antibiotic residues in eggs. A microbiological kit (Explorer® 2.0 test (Zeu Inmunotech, Spain)) and an immunobiosensor kit (Microarray II (AM® II) on Evidence Investigator™ system (Randox, UK)) have been evaluated and validated for screening of antibiotic residues in eggs, according to the European decision EC/2002/657 and to the European guideline for the validation of screening methods. The e-reader™ system, a new automatic incubator/reading system, was coupled to the Explorer 2.0 test. The AM II kit can detect residues of six different families of antibiotics in different matrices including eggs. For both tests, a different liquid/liquid extraction of eggs had to be developed. Specificities of the Explorer 2.0 and AM II kit were equal to 8% and 0% respectively. The detection capabilities were determined for 19 antibiotics, with representatives from different families, for Explorer 2.0 and 12 antibiotics for the AM II kit. For the nine antibiotics having a maximum residue limit (MRL) in eggs, the detection capabilities CCβ of Explorer 2.0 were below the MRL for four antibiotics, equal to the MRL for two antibiotics and between 1 and 1.5 MRLs for the three remaining antibiotics (tetracyclines). For the antibiotics from other families, the detection capabilities were low for beta-lactams and sulfonamides and satisfactory for dihydrostreptomycin (DHS) and fluoroquinolones, which are usually difficult to detect with microbiological tests. The CCβ values of the AM II kit were much lower than the respective MRLs for three detected antibiotics (tetracycline, oxytetracycline, tylosin). Concerning the nine other antibiotics, the detection capabilities determined were low. The highest CCβ was obtained for streptomycin (100 µg kg -1 ).

  2. Dissipation of chlorantraniliprole, chlorpyrifos-methyl and indoxacarb-insecticides used to control codling moth (Cydia Pomonella L.) and leafrollers (Tortricidae) in apples for production of baby food.

    PubMed

    Szpyrka, Ewa; Matyaszek, Aneta; Słowik-Borowiec, Magdalena

    2017-05-01

    Dissipations of three insecticides: chlorantraniliprole, chlorpyrifos-methyl and indoxacarb in apples were studied following their foliar application on apples intended for production of baby food. The apples were sprayed with formulations for control of codling moth (Cydia Pomonella L.) and leafrollers (Tortricidae). Six experiments were conducted; each insecticide was applied individually on dessert apples. A validated gas chromatography-based method with simultaneous electron capture and nitrogen-phosphorus detection (GC-ECD/NPD) was used for the residue analysis. The analytical performance of the method was satisfactory, with expanded uncertainties ≤36% (a coverage factor, k = 2, and a confidence level of 95%). The dissipations of insecticides were studied in pseudo-first-order kinetic models (for which the coefficient of determination, R 2 , ranged between 0.9188 and 0.9897). Residues of studied insecticides were below their maximum residue limits of 0.5 mg/kg at an early stage of growth of the fruit. The half-lives of chlorantraniliprole, chlorpyrifos-methyl and indoxacarb were 16-17, 4-6 and 20-24 days, respectively. The initial residue levels declined gradually and reached the level of 0.01 mg/kg in 1 month for chlorpyrifos-methyl, 2 months for chlorantraniliprole and 2.5 months for indoxacarb. To obtain the insecticide residue levels below 0.01 mg/kg, which is the default MRL for food intended for infants and young children, the application of the studied insecticides should be carried out at recommended doses not later then: 1 month before harvest for chlorpyrifos-methyl, 2 months for chlorantraniliprole and 2.5 months for indoxacarb.

  3. Alginate beads containing water treatment residuals for arsenic removal from water-formation and adsorption studies.

    PubMed

    Ociński, Daniel; Jacukowicz-Sobala, Irena; Kociołek-Balawejder, Elżbieta

    2016-12-01

    Water treatment residuals (WTRs) produced in large quantities during deironing and demanganization of infiltration water, due to high content of iron and manganese oxides, exhibit excellent sorptive properties toward arsenate and arsenite. Nonetheless, since they consist of microparticles, their practical use as an adsorbent is limited by difficulties with separation from treated solutions. The aim of this study was entrapment of chemically pretreated WTR into calcium alginate polymer and examination of sorptive properties of the obtained composite sorbent toward As(III) and As(V). Different products were formed varying in WTR content as well as in density of alginate matrix. In order to determine the key parameters of the adsorption process, both equilibrium and kinetic studies were conducted. The best properties were exhibited by a sorbent containing 5 % residuals, formed in alginate solution with a concentration of 1 %. In slightly acidic conditions (pH 4.5), its maximum sorption capacity was 3.4 and 2.9 mg g -1 for As(III) and As(V), respectively. At neutral pH, the adsorption effectiveness decreased to 3.3 mg As g -1 for arsenites and to 0.7 mg As g -1 for arsenates. The presence of carboxylic groups in polymer chains impeded in neutral conditions the diffusion of anions into sorbent beads; therefore, the main rate-limiting step of the adsorption, mainly in the case of arsenates, was intraparticle diffusion. The optimal condition for simultaneous removal of arsenates and arsenites from water by means of the obtained composite sorbent is slightly acidic pH, ensuring similar adsorption effectiveness for both arsenic species.

  4. Depletion of penicillin G residues in heavy sows after intramuscular injection. Part I: Tissue residue depletion

    USDA-ARS?s Scientific Manuscript database

    Heavy sows (n=126) were treated with penicillin G procaine at a 5x label dose (33,000 IU/kg) for 3 consecutive days by intramuscular (IM) injection using 3 separate patterns (treatments) of drug administration (42 sows per treatment). Treatments differed by pattern and maximum injection volume per s...

  5. Performance of blue-yellow screening test for antimicrobial detection in ovine milk.

    PubMed

    Linage, B; Gonzalo, C; Carriedo, J A; Asensio, J A; Blanco, M A; De La Fuente, L F; San Primitivo, F

    2007-12-01

    Drug residues in milk are important because of public health and industrial implications. The detection limits of 25 antimicrobial agents were determined by the blue-yellow screening method in ovine milk. For each drug, 8 concentrations were tested on 20 ovine milk samples from individual ewes in midlactation. Detection limits determined by means of logistic regression were below European Union maximum residue limits (EU-MRL) for penicillin G (3 to 4 microg/kg), ceftiofur (96 to 107 microg/kg), framycetin (720 to 781 microg/kg), neomycin (915 to 1,084 microg/kg), and tylosin (44 to 51 microg/kg). Detection limits for ampicillin (5 to 6 microg/kg), cloxacillin (33 to 42 microg/kg), cefoperazone (73 to 82 microg/kg), cefalexin (160 to 202 microg/kg), gentamycin (355 to 382 microg/kg), streptomycin (3,063 to 3,593 microg/kg), tilmicosin (109 to 131 microg/kg), erythromycin (444 to 522 microg/kg), spyramicin (1,106 to 1,346 microg/kg), sulfadimethoxine (101 to 119 microg/kg), sulfathiazole (122 to 151 microg/kg), sulfamethazine (309 to 328 microg/kg), sulfanilamide (1,750 to 2,674 microg/kg), tetracycline (233 to 257 microg/kg), oxytetracycline (398 to 501 microg/kg), doxycycline (323 to 419 microg/kg), chlortetracycline (3,331 to 3,989 microg/kg), danofloxacin (4.7 to 5.5 mg/kg), enrofloxacin (41 to 46 mg/kg), and flumequin (63 to 71 mg/kg) were higher than the EU-MRL. Although the blue-yellow method showed improved sensitivity compared with other tests studied in ovine milk, the performance of screening methods for detecting antimicrobial agents in milk of this species should be improved.

  6. Worldwide Regulations of Standard Values of Pesticides for Human Health Risk Control: A Review.

    PubMed

    Li, Zijian; Jennings, Aaron

    2017-07-22

    Abstract : The impact of pesticide residues on human health is a worldwide problem, as human exposure to pesticides can occur through ingestion, inhalation, and dermal contact. Regulatory jurisdictions have promulgated the standard values for pesticides in residential soil, air, drinking water, and agricultural commodity for years. Until now, more than 19,400 pesticide soil regulatory guidance values (RGVs) and 5400 pesticide drinking water maximum concentration levels (MCLs) have been regulated by 54 and 102 nations, respectively. Over 90 nations have provided pesticide agricultural commodity maximum residue limits (MRLs) for at least one of the 12 most commonly consumed agricultural foods. A total of 22 pesticides have been regulated with more than 100 soil RGVs, and 25 pesticides have more than 100 drinking water MCLs. This research indicates that those RGVs and MCLs for an individual pesticide could vary over seven (DDT drinking water MCLs), eight (Lindane soil RGVs), or even nine (Dieldrin soil RGVs) orders of magnitude. Human health risk uncertainty bounds and the implied total exposure mass burden model were applied to analyze the most commonly regulated and used pesticides for human health risk control. For the top 27 commonly regulated pesticides in soil, there are at least 300 RGVs (8% of the total) that are above all of the computed upper bounds for human health risk uncertainty. For the top 29 most-commonly regulated pesticides in drinking water, at least 172 drinking water MCLs (5% of the total) exceed the computed upper bounds for human health risk uncertainty; while for the 14 most widely used pesticides, there are at least 310 computed implied dose limits (28.0% of the total) that are above the acceptable daily intake values. The results show that some worldwide standard values were not derived conservatively enough to avoid human health risk by the pesticides, and that some values were not computed comprehensively by considering all major human exposure pathways.

  7. DDTs in mothers' milk, placenta and hair, and health risk assessment for infants at two coastal and inland cities in China.

    PubMed

    Man, Yu Bon; Chan, Janet Kit Yan; Wang, Hong Sheng; Wu, Sheng Chun; Wong, Ming Hung

    2014-04-01

    This study is a one of the very few investigating the dichloro-diphenyl-trichloroethanes (DDTs) (summation of o,p'-DDE, p,p'-DDE, o,p'-DDD, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in multiple human matrices in mothers' milk, placenta and hair collected from residents from two coastal cities: Guiyu (GY) and Taizhou (TZ) and one inland city: Lin'an (LA). TZ (milk: 360±319ng/g lipid wt.) showed significantly higher concentrations of DDTs than those from LA (milk: 190±131ng/g lipid wt.), whereas, concentrations of DDTs in GY (milk: 305±109ng/g lipid wt.) were in between TZ and LA. In addition, levels of DDTs in the human tissues from TZ (placenta: 122±109ng/g lipid wt.; hair: 79.9±215ng/g dry wt.) were significantly higher than those from Lin'an (placenta: 49.2±30.2ng/g lipid wt.; hair: 10.8±7.09ng/g dry wt.). The above concentrations of DDTs in milk exceeded the Codex Maximum Residue Limits/Extraneous Maximum Residue Limits for milk (20ng/g lipid wt. whole milk), indicating that the human milk samples were grossly polluted. The present study revealed that human specimens collected from the coastal city (TZ) were more contaminated with inland one (LA), based on the levels of DDTs contained in samples which may be due to the higher dietary exposure to DDTs via consumption of contaminated seafood. The estimated daily intakes of DDTs by GY, TZ and LA infants were 1.69±1.86, 1.48±0.79, and 0.95±0.73μg/kg body wt./day, respectively which did not exceed 10μg/kg body wt./day, the provisional tolerable daily intake proposed by the Food and Agriculture Organization/World Health Organization. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Worldwide Regulations of Standard Values of Pesticides for Human Health Risk Control: A Review

    PubMed Central

    Jennings, Aaron

    2017-01-01

    The impact of pesticide residues on human health is a worldwide problem, as human exposure to pesticides can occur through ingestion, inhalation, and dermal contact. Regulatory jurisdictions have promulgated the standard values for pesticides in residential soil, air, drinking water, and agricultural commodity for years. Until now, more than 19,400 pesticide soil regulatory guidance values (RGVs) and 5400 pesticide drinking water maximum concentration levels (MCLs) have been regulated by 54 and 102 nations, respectively. Over 90 nations have provided pesticide agricultural commodity maximum residue limits (MRLs) for at least one of the 12 most commonly consumed agricultural foods. A total of 22 pesticides have been regulated with more than 100 soil RGVs, and 25 pesticides have more than 100 drinking water MCLs. This research indicates that those RGVs and MCLs for an individual pesticide could vary over seven (DDT drinking water MCLs), eight (Lindane soil RGVs), or even nine (Dieldrin soil RGVs) orders of magnitude. Human health risk uncertainty bounds and the implied total exposure mass burden model were applied to analyze the most commonly regulated and used pesticides for human health risk control. For the top 27 commonly regulated pesticides in soil, there are at least 300 RGVs (8% of the total) that are above all of the computed upper bounds for human health risk uncertainty. For the top 29 most-commonly regulated pesticides in drinking water, at least 172 drinking water MCLs (5% of the total) exceed the computed upper bounds for human health risk uncertainty; while for the 14 most widely used pesticides, there are at least 310 computed implied dose limits (28.0% of the total) that are above the acceptable daily intake values. The results show that some worldwide standard values were not derived conservatively enough to avoid human health risk by the pesticides, and that some values were not computed comprehensively by considering all major human exposure pathways. PMID:28737697

  9. Rosin-enabled ultraclean and damage-free transfer of graphene for large-area flexible organic light-emitting diodes

    PubMed Central

    Zhang, Zhikun; Du, Jinhong; Zhang, Dingdong; Sun, Hengda; Yin, Lichang; Ma, Laipeng; Chen, Jiangshan; Ma, Dongge; Cheng, Hui-Ming; Ren, Wencai

    2017-01-01

    The large polymer particle residue generated during the transfer process of graphene grown by chemical vapour deposition is a critical issue that limits its use in large-area thin-film devices such as organic light-emitting diodes. The available lighting areas of the graphene-based organic light-emitting diodes reported so far are usually <1 cm2. Here we report a transfer method using rosin as a support layer, whose weak interaction with graphene, good solubility and sufficient strength enable ultraclean and damage-free transfer. The transferred graphene has a low surface roughness with an occasional maximum residue height of about 15 nm and a uniform sheet resistance of 560 Ω per square with about 1% deviation over a large area. Such clean, damage-free graphene has produced the four-inch monolithic flexible graphene-based organic light-emitting diode with a high brightness of about 10,000 cd m−2 that can already satisfy the requirements for lighting sources and displays. PMID:28233778

  10. Mixed culture polyhydroxyalkanoates production from sugar molasses: the use of a 2-stage CSTR system for culture selection.

    PubMed

    Albuquerque, M G E; Concas, S; Bengtsson, S; Reis, M A M

    2010-09-01

    Polyhydroxyalkanoates (PHAs) are promising biodegradable polymers. The use of mixed microbial cultures (MMC) and low cost feedstocks have a positive impact on the cost-effectiveness of the process. It has typically been carried out in Sequencing Batch Reactors (SBR). In this study, a 2-stage CSTR system (under Feast and Famine conditions) was used to effectively select for PHA-storing organisms using fermented molasses as feedstock. The effect of influent substrate concentration (60-120 Cmmol VFA/L) and HRT ratio between the reactors (0.2-0.5h/h) on the system's selection efficiency was assessed. It was shown that Feast reactor residual substrate concentration impacted on the selective pressure for PHA storage (due to substrate-dependent kinetic limitation). Moreover, a residual substrate concentration coming from the Feast to the Famine reactor did not jeopardize the physiological adaptation required for enhanced PHA storage. The culture reached a maximum PHA content of 61%. This success opens new perspectives to the use of wastewater treatment infrastructure for PHA production, thus valorizing either excess sludge or wastewaters. Copyright 2010 Elsevier Ltd. All rights reserved.

  11. Aluminum drinking water treatment residuals (Al-WTRs) as sorbent for mercury: Implications for soil remediation.

    PubMed

    Hovsepyan, Anna; Bonzongo, Jean-Claude J

    2009-05-15

    The potential of readily available and non-hazardous waste material, aluminum drinking water treatment residuals (Al-WTRs), to efficiently sorb and immobilize mercury (Hg) from aqueous solutions was evaluated. Al-WTR samples with average specific surface area of 48m(2)/g and internal micropore surface area of 120m(2)/g were used in a series of batch sorption experiments. Obtained sorption isotherms indicated a strong affinity of Hg for Al-WTRs. Using the Langmuir adsorption model, a relatively high maximum sorption capacity of 79mg Hg/g Al-WTRs was determined. Sorption kinetic data was best fit to a pseudo-first-order model, while the use of the Weber-Morris and Bangham models suggested that the intraparticle diffusion could be the rate-limiting step. Also, Al-WTRs effectively immoblized Hg in the pH range of 3-8. The results from these short-term experiments demonstrate that Al-WTRs can be effectively used to remove Hg from aqueous solutions. This ability points to the potential of Al-WTRs as a sorbent in soil remediation techniques based on Hg-immobilization.

  12. Environmental status of groundwater affected by chromite ore processing residue (COPR) dumpsites during pre-monsoon and monsoon seasons.

    PubMed

    Matern, Katrin; Weigand, Harald; Singh, Abhas; Mansfeldt, Tim

    2017-02-01

    Chromite ore processing residue (COPR) is generated by the roasting of chromite ores for the extraction of chromium. Leaching of carcinogenic hexavalent chromium (Cr(VI)) from COPR dumpsites and contamination of groundwater is a key environmental risk. The objective of the study was to evaluate Cr(VI) contamination in groundwater in the vicinity of three COPR disposal sites in Uttar Pradesh, India, in the pre-monsoon and monsoon seasons. Groundwater samples (n = 57 pre-monsoon, n = 70 monsoon) were taken in 2014 and analyzed for Cr(VI) and relevant hydrochemical parameters. The site-specific ranges of Cr(VI) concentrations in groundwater were <0.005 to 34.8 mg L -1 (Rania), <0.005 to 115 mg L -1 (Chhiwali), and <0.005 to 2.0 mg L -1 (Godhrauli). Maximum levels of Cr(VI) were found close to the COPR dumpsites and significantly exceeded safe drinking water limits (0.05 mg L -1 ). No significant dependence of Cr(VI) concentration on monsoons was observed.

  13. Dissipation Pattern, Processing Factors, and Safety Evaluation for Dimethoate and Its Metabolite (Omethoate) in Tea (Camellia Sinensis)

    PubMed Central

    Pan, Rong; Chen, Hong-Ping; Zhang, Ming-Lu; Wang, Qing-Hua; Jiang, Ying; Liu, Xin

    2015-01-01

    Residue levels of dimethoate and its oxon metabolite (omethoate) during tea planting, manufacturing, and brewing were investigated using a modified QuEChERS sample preparation and gas chromatography. Dissipation of dimethoate and its metabolite in tea plantation followed the first-order kinetic with a half-life of 1.08–1.27 d. Tea manufacturing has positive effects on dimethoate dissipation. Processing factors of dimethoate are in the range of 2.11–2.41 and 1.41–1.70 during green tea and black tea manufacturing, respectively. Omethoate underwent generation as well as dissipation during tea manufacturing. Sum of dimethoate and omethoate led to a large portion of 80.5–84.9% transferring into tea infusion. Results of safety evaluation indicated that omethoate could bring higher human health risk than dimethoate due to its higher hazard quotient by drinking tea. These results would provide information for the establishment of maximum residue limit and instruction for the application of dimethoate formulation on tea crop. PMID:26406463

  14. Limited survey for the presence of aflatoxins in foods from local markets and supermarkets in Valencia, Spain.

    PubMed

    Blesa, J; Soriano, J M; Moltó, J C; Mañes, J

    2004-02-01

    Aflatoxin B1 (AFB1), B2 (AFB2), G1 (AFG1) and G2 (AFG2) were extracted by matrix solid-phase dispersion with C18 silica and acetonitrile as the eluting solvent, analysed by liquid chromatography with fluorescence detection and confirmed by liquid chromatography with mass spectrometry using an electrospray interface in 58 samples grouped as cereals, dried fruits, herbs and spices, pulses, snacks, and nuts and nut products collected from local markets and supermarkets in Valencia, Spain. All samples analysed by the proposed method were previously studied with an enzyme-linked immunosorbent assay as a screening protocol for the fast detection of mycotoxins. The samples containing residues (3/58) were hazelnut (0.42 and 0.52 microg kg(-1) for AFB1 and AFG1, respectively), nut cocktail (0.29 and 0.47 microg kg(-1) for AFB1 and AFG1, respectively) and pinhol (0.30 microg kg(-1) for AFG1). Such values were below the legislated maximum residue levels for the European Union.

  15. Effect of temperature (cooking and freezing) on the concentration of oxytetracycline residue in experimentally induced birds

    PubMed Central

    Vivienne, Ezenduka Ekene; Josephine, Okorie-kanu Onyinye; Anaelom, Nwanta John

    2018-01-01

    Aim: The objective of this study was to determine the effect of varying temperatures (different cooking methods and freezing) on the concentration of oxytetracycline (OTC) residues in tissues of broiler birds. Materials and Methods: Fifty, 5-week-old birds were purchased and acclimatized for 3 weeks while being fed antibiotic-free feed and water. Four birds were then tested for residue and in the absence; the remaining birds were injected intramuscularly with oxytetracycline at its therapeutic dose. Muscle and liver samples of the treated birds were harvested and checked for OTC residues before subjecting them to boiling, microwaving, and roasting. The three plate test was used for the residue detection. Result: OTC was detected at both pH 6.0 and pH 7.2 but not detected at pH 8.0. Roasting and boiling significantly reduced the concentration of oxytetracycline in muscle by 53.6% and 69.6%, respectively, at pH 6.0, microwaving reduced the concentration by 49.1% but was not statistically significant. The same pattern was followed at pH 7.2 with reduction of 34.3%, 53.2%, and 67.7% for microwaved, roasted, and boiled. For the liver tissues, there was a significant reduction in the concentration for both pH: 6.0 (57.75%, 79.75%, and 89%; pH 7.2 (48.06%, 79.6%, and 88.79%) for boiled, microwaved, and roasted samples. Boiling had a greater reduction effect for muscle samples while roasting had a greater reduction in liver samples at both pHs. Freezing at −10°C had no effect on the concentration of OTC even after 9 days. Conclusion: The significant reduction of OTC concentration by cooking indicates that consumers may not be at risk of the effects of OTC residues in meat, but microwaving meat may not reduce the concentration below the maximum residue limit if the initial concentration is very high. Therefore, routine monitoring of drug residues in farms and abattoirs is still advocated. PMID:29657398

  16. Multi-residue method for the determination of antibiotics and some of their metabolites in seafood.

    PubMed

    Serra-Compte, Albert; Álvarez-Muñoz, Diana; Rodríguez-Mozaz, Sara; Barceló, Damià

    2017-06-01

    The presence of antibiotics in seafood for human consumption may pose a risk for consumers. A methodology for the analysis of antibiotics in seafood based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction, followed by detection and quantification using liquid chromatography coupled to mass spectrometry was developed. The analytical method was evaluated for the determination of 23 antibiotics (including parent compounds and some metabolites) in fish, mussels and clams. Recoveries ranged between 30% and 70% for most of the compounds and method detection and quantification limits (MDLs and MQLs) were between 0.01 and 0.31 ng/g dry weigh (dw) and 0.02-1.03 ng/g (dw) respectively. Real seafood samples were analysed using this method. Nine antibiotics were found at levels above MDLs; however none of them exceed the maximum residue limits (MRL) established by the authorities. Tetracycline was the most ubiquitous compound, presenting also the highest concentration: 5.63 ng/g (dw) in fish from Netherlands. In addition, an alternative technique based on microbial growth inhibition was explored as semiquantitative detection method of antibiotics in seafood. This methodology could be applied as a fast screening technique for the detection of macrolides and β-lactams in seafood but further research is needed for other antibiotics families. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Point-of-care testing for streptomycin based on aptamer recognizing and digital image colorimetry by smartphone.

    PubMed

    Lin, Bixia; Yu, Ying; Cao, Yujuan; Guo, Manli; Zhu, Debin; Dai, Jiaxing; Zheng, Minshi

    2018-02-15

    The rapid detection of antibiotic residual in everyday life is very important for food safety. In order to realize the on-site and visual detection of antibiotic, a POCT method was established by using digital image colorimetry based on smartphone. Streptomycin was taken as the analyte model of antibiotics, streptomycin aptamer preferentially recognized analyte, and the excess aptamer hybridized with the complementary DNA to form the dsDNA. SYBR Green I combined with the dsDNA and then emitted obvious green fluorescence, thus the fluorescence intensity decreased with the increasing of streptomycin concentration. Then a smartphone-based device was constructed as the fluorescence readout. The smartphone camera acquired the images of the fluorescence derived from the samples, and the Touch Color APP installed in smartphone read out the RGB values of the images. There was a linear relationship between the G values and the streptomycin concentrations in the range of 0.1-100µM. The detection limit was 94nM, which was lower than the maximum residue limit defined by World Health Organization. The POCT method was applied for determining streptomycin in chicken and milk samples with recoveries in 94.1-110%. This method had the advantages of good selectivity, simple operation and on-site visualization. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry.

    PubMed

    Petrarca, Mateus Henrique; Ccanccapa-Cartagena, Alexander; Masiá, Ana; Godoy, Helena Teixeira; Picó, Yolanda

    2017-05-12

    A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some of them too high to meet the strict legislation regarding baby food. Nonetheless, the combination of ultrasound and DLLME also resulted in a high sample throughput and environmental-friendly method, whose LOQs were lower than the default maximum residue limit (MRL) of 10μgkg -1 set by European Community for baby foods. In the commercial baby foods analyzed, cyhalothrin and etofenprox were detected in different samples, demonstrating the suitability of proposed method for baby food control. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Baseline levels of melamine in food items sold in Canada. II. Egg, soy, vegetable, fish and shrimp products.

    PubMed

    Tittlemier, Sheryl A; Lau, Benjamin P-Y; Ménard, Cathie; Corrigan, Catherine; Sparling, Melissa; Gaertner, Dean; Cao, Xu-Liang; Dabeka, Bob; Hilts, Carla

    2010-01-01

    A variety of egg-containing, soy-based, fish, shrimp and vegetable products sold in Canada were analysed for melamine (MEL) using a sensitive solid-phase extraction LC-MS/MS analytical method. MEL was detected above the method quantification limit of 0.004 mg/kg in 98 of the 378 samples analysed. Concentrations in the various food product groups ranged 0.00507-0.247 mg/kg (egg-containing items), 0.00408-0.0479 mg/kg (soy-based meat substitutes), 0.00409-1.10 mg/kg (fish and shrimp products), and 0.00464-0.688 mg/kg (vegetable products). MEL was detected less frequently in egg- and soy-containing products. The presence of MEL in most of the Canadian Total Diet Study shrimp composites collected after 2001 suggested the residues in shrimp were caused by a relatively recent exposure to MEL. All concentrations of MEL reported were lower than the 2.5 mg/kg interim standard established for MEL in items containing milk and milk-derived ingredients and the respective maximum residue limits for cyromazine and its metabolite, melamine, in vegetables set by the Canadian Government (2009; http://www.hc-sc.gc.ca/fn-an/securit/chem-chim/melamine/qa-melamine-qr-eng.php#8 ). The consumption of foods containing these low levels of MEL does not constitute a health risk for consumers.

  20. Assessing item fit for unidimensional item response theory models using residuals from estimated item response functions.

    PubMed

    Haberman, Shelby J; Sinharay, Sandip; Chon, Kyong Hee

    2013-07-01

    Residual analysis (e.g. Hambleton & Swaminathan, Item response theory: principles and applications, Kluwer Academic, Boston, 1985; Hambleton, Swaminathan, & Rogers, Fundamentals of item response theory, Sage, Newbury Park, 1991) is a popular method to assess fit of item response theory (IRT) models. We suggest a form of residual analysis that may be applied to assess item fit for unidimensional IRT models. The residual analysis consists of a comparison of the maximum-likelihood estimate of the item characteristic curve with an alternative ratio estimate of the item characteristic curve. The large sample distribution of the residual is proved to be standardized normal when the IRT model fits the data. We compare the performance of our suggested residual to the standardized residual of Hambleton et al. (Fundamentals of item response theory, Sage, Newbury Park, 1991) in a detailed simulation study. We then calculate our suggested residuals using data from an operational test. The residuals appear to be useful in assessing the item fit for unidimensional IRT models.

  1. The two-phase flow IPTT method for measurement of nonwetting-wetting liquid interfacial areas at higher nonwetting saturations in natural porous media

    PubMed Central

    Zhong, Hua; Ouni, Asma El; Lin, Dan; Wang, Bingguo; Brusseau, Mark L

    2017-01-01

    Interfacial areas between nonwetting-wetting (NW-W) liquids in natural porous media were measured using a modified version of the interfacial partitioning tracer test (IPTT) method that employed simultaneous two-phase flow conditions, which allowed measurement at NW saturations higher than trapped residual saturation. Measurements were conducted over a range of saturations for a well-sorted quartz sand under three wetting scenarios of primary drainage (PD), secondary imbibition (SI), and secondary drainage (SD). Limited sets of experiments were also conducted for a model glass-bead medium and for a soil. The measured interfacial areas were compared to interfacial areas measured using the standard IPTT method for liquid-liquid systems, which employs residual NW saturations. In addition, the theoretical maximum interfacial areas estimated from the measured data are compared to specific solid surface areas measured with the N2/BET method and estimated based on geometrical calculations for smooth spheres. Interfacial areas increase linearly with decreasing water saturation over the range of saturations employed. The maximum interfacial areas determined for the glass beads, which have no surface roughness, are 32±4 and 36±5 cm−1 for PD and SI cycles, respectively. The values are similar to the geometric specific solid surface area (31±2 cm−1) and the N2/BET solid surface area (28±2 cm−1). The maximum interfacial areas are 274±38, 235±27, and 581±160 cm−1 for the sand for PD, SI, and SD cycles, respectively, and ~7625 cm−1 for the soil for PD and SI. The maximum interfacial areas for the sand and soil are significantly larger than the estimated smooth-sphere specific solid surface areas (107±8 cm−1 and 152±8 cm−1, respectively), but much smaller than the N2/BET solid surface area (1387±92 cm−1 and 55224 cm−1, respectively). The NW-W interfacial areas measured with the two-phase flow method compare well to values measured using the standard IPTT method. PMID:28959079

  2. Determination of the residue levels of nicarbazin and combination nicarbazin-narasin in broiler chickens after oral administration

    PubMed Central

    da Silva, Guilherme Resende; de Assis, Débora Cristina Sampaio; Cançado, Silvana de Vasconcelos

    2017-01-01

    The depletion times of the anticoccidial nicarbazin administered individually and of nicarbazin and narasin administered in combination were evaluated by determining the presence and levels of 4,4'-dinitrocarbanilide (DNC), the marker residue for nicarbazin, and narasin residues in the muscle tissues of broiler chickens subjected to a pharmacological treatment. A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was used. The results showed the presence of all anticoccidial residues; however, the DNC levels were higher when the nicarbazin was administered individually than when it was used in association with narasin throughout the experimental period. After six days of withdrawal, the DNC level following nicarbazin administration alone was lower than the maximum residue level (MRL) of 200 μg kg-1. However, when the nicarbazin was co-administered with narasin, the concentrations of DNC were lower than the MRL after four days of withdrawal. These results may be justified because the dosage of nicarbazin, when administrated individually, is greater than when it is used in combination with narasin. The levels of narasin were lower than the MRL of 15 μg kg-1 throughout the evaluation period. It was concluded that nicarbazin is rapidly metabolized from the broiler muscles up to six days of withdrawal since the DNC levels were lower than the maximum residue level (MRL) and the concentrations of narasin were lower than the MRL throughout the evaluation period. PMID:28750013

  3. Azinphos-methyl residues in apples and spatial distribution of fluorescein in vase-shaped apple trees.

    PubMed

    Bélanger, A; Bostanian, N J; Boivin, G; Boudreau, F

    1991-06-01

    Vase-shaped standard apple trees cv. McIntosh were sprayed with azinphos-methyl at pink, pink and 1st cover and 1st cover only. Residue analyses by gas chromatography revealed detectable residues on foliage until mid summer. At harvest, negligible residue levels were found on the peel and the whole apple. On four trees, fluorescein was sprayed in the same manner as the insecticide and maximum levels of the dye were detected on the outside lower canopy along the row. Minimal concentration of fluorescein was detected on the inner upper canopy away from the direction of the row.

  4. Development of an analytical method for analysis of flubendiamide, des-iodo flubendiamide and study of their residue persistence in tomato and soil.

    PubMed

    Mohapatra, S; Ahuja, A K; Deepa, M; Jagadish, G K; Rashmi, N; Sharma, D

    2011-01-01

    Flubendiamide is a new insecticide that has been found to give excellent control of lepidopterous pests of tomato. This study has been undertaken to develop an improved method for analysis of flubendiamide and its metabolite des-iodo flubendiamide and determine residue retention in tomato and soil. The analytical method developed involved extraction of flubendiamide and its metabolite des-iodo flubendiamide with acetonitrile, liquid-liquid partitioning into hexane-ethyl acetate mixture (6:4, v v⁻¹) and cleanup with activated neutral alumina. Finally the residues were dissolved in gradient high pressure liquid chromatography (HPLC) grade acetonitrile for analysis by HPLC. The mobile phase, acetonitrile-water at 60:40 (v v⁻¹) proportion and the wavelength of 235 nm gave maximum peak resolution. Using the above method and HPLC parameters described, nearly 100 % recovery of both insecticides were obtained. There was no matrix interference and the limit of quantification (LOQ) of the method was 0.01 mg kg⁻¹. Initial residue deposits of flubendiamide on field-treated tomato from treatments @ 48 and 96 g active ingredient hectare⁻¹ were 0.83 and 1.68 mg kg⁻¹, respectively. The residues of flubendiamide dissipated at the half-life of 3.9 and 4.4 days from treatments @ 48 and 96 g a.i. ha⁻¹, respectively and persisted for 15 days from both the treatments. Des-iodo flubendiamide was not detected in tomato fruits at any time during the study period. Residues of flubendiamide and des-iodo flubendiamide in soil from treatment @ 48 and 96 g a.i. ha⁻¹ were below detectable level (BDL, < 0.01 mg kg⁻¹) after 20 days. Flubendiamide completely dissipated from tomato within 20 days when the 480 SC formulation was applied at doses recommended for protection against lepidopterous pests.

  5. 14 CFR 25.1505 - Maximum operating limit speed.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 14 Aeronautics and Space 1 2010-01-01 2010-01-01 false Maximum operating limit speed. 25.1505... Operating Limitations § 25.1505 Maximum operating limit speed. The maximum operating limit speed (V MO/M MO airspeed or Mach Number, whichever is critical at a particular altitude) is a speed that may not be...

  6. 14 CFR 25.1505 - Maximum operating limit speed.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 14 Aeronautics and Space 1 2011-01-01 2011-01-01 false Maximum operating limit speed. 25.1505... Operating Limitations § 25.1505 Maximum operating limit speed. The maximum operating limit speed (V MO/M MO airspeed or Mach Number, whichever is critical at a particular altitude) is a speed that may not be...

  7. Weight History, All-Cause and Cause-Specific Mortality in Three Prospective Cohort Studies

    PubMed Central

    Yu, Edward; Stokes, Andrew C.; Ley, Sylvia H.; Manson, JoAnn E.; Willett, Walter; Satija, Ambika; Hu, Frank B.

    2017-01-01

    BACKGROUND The relationship between body mass index (BMI) and mortality remains controversial. OBJECTIVE To investigate the relationship between maximum BMI over 16 years and subsequent mortality. DESIGN Three prospective cohort studies. SETTING Nurses’ Health Study I and II, Health Professionals Follow-up Study. PARTICIPANTS 225,072 men and women accruing 32,571 deaths over a mean of 12.3 years of follow-up. MEASUREMENTS Maximum BMI over 16 years of weight history and all-cause and cause-specific mortality. RESULTS Maximum BMIs in the overweight (25.0 to 29.9 kg/m2) (multivariate hazard ratio (HR), 1.06; 95% confidence interval (CI), 1.03 – 1.08), obese I (30.0 to 34.9 kg/m2), (HR, 1.24; 95% CI, 1.20 – 1.29), and obese II (≥ 35.0 kg/m2) (HR, 1.73; 95% CI, 1.66 – 1.80) categories were associated with increases in risk of all-cause mortality. The pattern of excess risk with a maximum BMI above normal weight was maintained across strata defined by smoking status, sex, and age, but the excess was greatest among those <70 years old and never smokers. In contrast, a significant inverse association between overweight and mortality (HR, 0.96; 95% CI, 0.94 – 0.99) was observed when BMI was defined using a single baseline measurement. Maximum overweight was also associated with increased cause-specific mortality, including deaths from cardiovascular diseases and coronary heart disease. LIMITATIONS Residual confounding and misclassification. CONCLUSIONS The paradoxical association between overweight and mortality is reversed in analyses incorporating weight history. Maximum BMI may be a useful metric to minimize reverse causation bias associated with a single baseline BMI assessment. PMID:28384755

  8. Risk assessment and risk management at the Canadian Food Inspection Agency (CFIA): a perspective on the monitoring of foods for chemical residues.

    PubMed

    Bietlot, Henri P; Kolakowski, Beata

    2012-08-01

    The Canadian Food Inspection Agency (CFIA) uses 'Ranked Risk Assessment' (RRA) to prioritize chemical hazards for inclusion in monitoring programmes or method development projects based on their relative risk. The relative risk is calculated for a chemical by scoring toxicity and exposure in the 'risk model scoring system' of the Risk Priority Compound List (RPCL). The relative ranking and the risk management options are maintained and updated in the RPCL. The ranking may be refined by the data generated by the sampling and testing programs. The two principal sampling and testing programmes are the National Chemical Residue Monitoring Program (NCRMP) and the Food Safety Action Plan (FSAP). The NCRMP sampling plans focus on the analysis of federally registered products (dairy, eggs, honey, meat and poultry, fresh and processed fruit and vegetable commodities, and maple syrup) for residues of veterinary drugs, pesticides, environmental contaminants, mycotoxins, and metals. The NCRMP is complemented by the Food Safety Action Plan (FSAP) targeted surveys. These surveys focus on emerging chemical hazards associated with specific foods or geographical regions for which applicable maximum residue limits (MRLs) are not set. The data from the NCRMP and FSAP also influence the risk management (follow-up) options. Follow-up actions vary according to the magnitude of the health risk, all with the objective of preventing any repeat occurrence to minimize consumer exposure to a product representing a potential risk to human health. © Her Majesty the Queen in Right of Canada 2012. Drug Testing and Analysis © 2012 John Wiley & Sons, Ltd.

  9. Food safety in Thailand 1: it is safe to eat watermelon and durian in Thailand.

    PubMed

    Wanwimolruk, Sompon; Kanchanamayoon, Onnicha; Boonpangrak, Somchai; Prachayasittikul, Virapong

    2015-05-01

    The wide use of pesticides raises serious concerns regarding food safety and environmental impacts. There is increasing public concern about the potential health risks linked with exposure to pesticides. Regulation of maximum residue limits (MRL) of pesticide residues in food commodities has been established in many developed countries. For developing countries, like Thailand, this regulation often exists in law, but is not completely enforced in practice. Thus, pesticide residue levels in vegetables and fruits have not been thoroughly monitored. The present study aimed to examine potential health risks associated with pesticide exposure by determining the pesticide residues in two commonly consumed fruits, watermelon and durian. The fruit samples were purchased from markets in central provinces of Thailand and assayed for the content of 28 pesticides. Analysis of pesticides was performed by multiresidue extraction and followed by GC-MS/MS detection. Of 28 pesticides investigated, 5 were detected in 90.7% of the watermelon samples (n = 75) and 3 in 90% of durian samples (n = 30). Carbofuran, chlorpyrifos, diazinon, dimethoate and metalaxyl were found in watermelons, whereas dichlorvos, dimethoate and metalaxyl were detected in durians. However, their levels were much lower than the recommended MRL values. These pesticide levels detected in the fruits are unlikely to harm the consumers; therefore it is safe to eat watermelon and durian in Thailand. While our results found negligible risk associated with pesticide exposure from consuming these common tropical fruits, special precautions should be considered to decrease total exposure to these harmful pesticides from various foods.

  10. Electrochemical Quartz Crystal Nanobalance (EQCN) Based Biosensor for Sensitive Detection of Antibiotic Residues in Milk.

    PubMed

    Bhand, Sunil; Mishra, Geetesh K

    2017-01-01

    An electrochemical quartz crystal nanobalance (EQCN), which provides real-time analysis of dynamic surface events, is a valuable tool for analyzing biomolecular interactions. EQCN biosensors are based on mass-sensitive measurements that can detect small mass changes caused by chemical binding to small piezoelectric crystals. Among the various biosensors, the piezoelectric biosensor is considered one of the most sensitive analytical techniques, capable of detecting antigens at picogram levels. EQCN is an effective monitoring technique for regulation of the antibiotics below the maximum residual limit (MRL). The analysis of antibiotic residues requires high sensitivity, rapidity, reliability and cost effectiveness. For analytical purposes the general approach is to take advantage of the piezoelectric effect by immobilizing a biosensing layer on top of the piezoelectric crystal. The sensing layer usually comprises a biological material such as an antibody, enzymes, or aptamers having high specificity and selectivity for the target molecule to be detected. The biosensing layer is usually functionalized using surface chemistry modifications. When these bio-functionalized quartz crystals are exposed to a particular substance of interest (e.g., a substrate, inhibitor, antigen or protein), binding interaction occurs. This causes a frequency or mass change that can be used to determine the amount of material interacted or bound. EQCN biosensors can easily be automated by using a flow injection analysis (FIA) setup coupled through automated pumps and injection valves. Such FIA-EQCN biosensors have great potential for the detection of different analytes such as antibiotic residues in various matrices such as water, waste water, and milk.

  11. Residual stress and damage-induced critical fracture on CO2 laser treated fused silica

    NASA Astrophysics Data System (ADS)

    Matthews, M. J.; Stolken, J. S.; Vignes, R. M.; Norton, M. A.; Yang, S.; Cooke, J. D.; Guss, G. M.; Adams, J. J.

    2009-10-01

    Localized damage repair and polishing of silica-based optics using mid- and far-IR CO2 lasers has been shown to be an effective method for increasing optical damage threshold in the UV. However, it is known that CO2 laser heating of silicate surfaces can lead to a level of residual stress capable of causing critical fracture either during or after laser treatment. Sufficient control of the surface temperature as a function of time and position is therefore required to limit this residual stress to an acceptable level to avoid critical fracture. In this work we present the results of 351 nm, 3ns Gaussian damage growth experiments within regions of varying residual stress caused by prior CO2 laser exposures. Thermally stressed regions were non-destructively characterized using polarimetry and confocal Raman microscopy to measure the stress induced birefringence and fictive temperature respectively. For 1~40s square pulse CO2 laser exposures created over 0.5-1.25kW/cm2 with a 1-3mm 1/e2 diameter beam (Tmax~1500-3000K), the critical damage site size leading to fracture increases weakly with peak temperature, but shows a stronger dependence on cooling rate, as predicted by finite element hydrodynamics simulations. Confocal micro-Raman was used to probe structural changes to the glass over different thermal histories and indicated a maximum fictive temperature of 1900K for Tmax>=2000K. The effect of cooling rate on fictive temperature caused by CO2 laser heating are consistent with finite element calculations based on a Tool-Narayanaswamy relaxation model.

  12. Effect of individual parameter changes on the outcome of the estimated short-term dietary exposure to pesticides.

    PubMed

    van der Velde-Koerts, Trijntje; Breysse, Nicolas; Pattingre, Lauriane; Hamey, Paul Y; Lutze, Jason; Mahieu, Karin; Margerison, Sam; Ossendorp, Bernadette C; Reich, Hermine; Rietveld, Anton; Sarda, Xavier; Vial, Gaelle; Sieke, Christian

    2018-06-03

    In 2015 a scientific workshop was held in Geneva, where updating the International Estimate of Short-Term Intake (IESTI) equations was suggested. This paper studies the effects of the proposed changes in residue inputs, large portions, variability factors and unit weights on the overall short-term dietary exposure estimate. Depending on the IESTI case equation, a median increase in estimated overall exposure by a factor of 1.0-6.8 was observed when the current IESTI equations are replaced by the proposed IESTI equations. The highest increase in the estimated exposure arises from the replacement of the median residue (STMR) by the maximum residue limit (MRL) for bulked and blended commodities (case 3 equations). The change in large portion parameter does not have a significant impact on the estimated exposure. The use of large portions derived from the general population covering all age groups and bodyweights should be avoided when large portions are not expressed on an individual bodyweight basis. Replacement of the highest residue (HR) by the MRL and removal of the unit weight each increase the estimated exposure for small-, medium- and large-sized commodities (case 1, case 2a or case 2b equations). However, within the EU framework lowering of the variability factor from 7 or 5 to 3 counterbalances the effect of changes in other parameters, resulting in an estimated overall exposure change for the EU situation of a factor of 0.87-1.7 and 0.6-1.4 for IESTI case 2a and case 2b equations, respectively.

  13. Theory of Financial Risk and Derivative Pricing

    NASA Astrophysics Data System (ADS)

    Bouchaud, Jean-Philippe; Potters, Marc

    2009-01-01

    Foreword; Preface; 1. Probability theory: basic notions; 2. Maximum and addition of random variables; 3. Continuous time limit, Ito calculus and path integrals; 4. Analysis of empirical data; 5. Financial products and financial markets; 6. Statistics of real prices: basic results; 7. Non-linear correlations and volatility fluctuations; 8. Skewness and price-volatility correlations; 9. Cross-correlations; 10. Risk measures; 11. Extreme correlations and variety; 12. Optimal portfolios; 13. Futures and options: fundamental concepts; 14. Options: hedging and residual risk; 15. Options: the role of drift and correlations; 16. Options: the Black and Scholes model; 17. Options: some more specific problems; 18. Options: minimum variance Monte-Carlo; 19. The yield curve; 20. Simple mechanisms for anomalous price statistics; Index of most important symbols; Index.

  14. Theory of Financial Risk and Derivative Pricing - 2nd Edition

    NASA Astrophysics Data System (ADS)

    Bouchaud, Jean-Philippe; Potters, Marc

    2003-12-01

    Foreword; Preface; 1. Probability theory: basic notions; 2. Maximum and addition of random variables; 3. Continuous time limit, Ito calculus and path integrals; 4. Analysis of empirical data; 5. Financial products and financial markets; 6. Statistics of real prices: basic results; 7. Non-linear correlations and volatility fluctuations; 8. Skewness and price-volatility correlations; 9. Cross-correlations; 10. Risk measures; 11. Extreme correlations and variety; 12. Optimal portfolios; 13. Futures and options: fundamental concepts; 14. Options: hedging and residual risk; 15. Options: the role of drift and correlations; 16. Options: the Black and Scholes model; 17. Options: some more specific problems; 18. Options: minimum variance Monte-Carlo; 19. The yield curve; 20. Simple mechanisms for anomalous price statistics; Index of most important symbols; Index.

  15. Large-area sheet task advanced dendritic web growth development

    NASA Technical Reports Server (NTRS)

    Duncan, C. S.; Seidensticker, R. G.; Mchugh, J. P.

    1984-01-01

    The thermal models used for analyzing dendritic web growth and calculating the thermal stress were reexamined to establish the validity limits imposed by the assumptions of the models. Also, the effects of thermal conduction through the gas phase were evaluated and found to be small. New growth designs, both static and dynamic, were generated using the modeling results. Residual stress effects in dendritic web were examined. In the laboratory, new techniques for the control of temperature distributions in three dimensions were developed. A new maximum undeformed web width of 5.8 cm was achieved. A 58% increase in growth velocity of 150 micrometers thickness was achieved with dynamic hardware. The area throughput goals for transient growth of 30 and 35 sq cm/min were exceeded.

  16. Dissipation kinetics of bifenazate in tea under tropical conditions.

    PubMed

    Satheshkumar, Annamalai; Senthurpandian, Velu Kalaipandian; Shanmugaselvan, Veilumuthu Anandham

    2014-02-15

    Field experiments were conducted during April and May of 2011 in Valparai, Coonoor and Gudalur (Tamil Nadu, India) to determine the residues of bifenazate in black tea. From this study, residue levels of bifenazate at different harvest intervals, persistence, dissipation pattern during processing, rate constant and half-life values were calculated. Residues of bifenazate dissipated exponentially after spraying and at Gudalur trial, on the 16th day after application residues were below the maximum residue level of 0.02 mg/kg set by the European Union. However, no residues were detected in the tea brew. Regression lines drawn for bifenazate showed that it followed first order dissipation kinetics. Half-life values varied from 1.03 to 1.36 days for bifenazate and a pre-harvest interval of 16 days is suggested. Copyright © 2013 Elsevier Ltd. All rights reserved.

  17. Differences and similarities in fatigue behaviour and its influences on critical current and residual strength between Ti-Nb and Nb3Al superconducting composite wires

    NASA Astrophysics Data System (ADS)

    Ochiai, Shojiro; Oki, Yuichiro; Sekino, Fumiaki; Ohno, Hiroaki; Hojo, Masaki; Moriai, Hidezumi; Sakai, Shuji; Koganeya, Masanobu; Hayashi, Kazuhiko; Yamada, Yuichi; Ayai, Naoki; Watanabe, Kazuo

    2000-04-01

    The influences of fatigue damage introduced at room temperature on critical current at 4.2 K and residual strength at room temperature of Ti-Nb superconducting composite wire with a low copper ratio (1.04) were studied. The experimental results were compared with those of Nb3 Al composite. The following differences between the composites were found: the fracture surface of the Ti-Nb filaments in the composite varies from a ductile pattern under static loading to a brittle one under cyclic loading, while the Nb3 Al compound always shows a brittle pattern under both loadings; the fracture strength of the Ti-Nb composite is given by the net stress criterion but that of Nb3 Al by the stress intensity factor criterion; in the Ti-Nb composite the critical current Ic decreases with increasing number of stress cycles simultaneously with the residual strength icons/Journals/Common/sigma" ALT="sigma" ALIGN="TOP"/> c ,r , while in the Nb3 Al composite Ic decreases later than icons/Journals/Common/sigma" ALT="sigma" ALIGN="TOP"/> c ,r . On the other hand, both composites have the following similarities: the filaments are fractured due to the propagation of the fatigue crack nucleated in the copper; with increasing number of stress cycles, the damage progresses in the order of stage I (formation of cracks in the clad copper), stage II (stable propagation of the fatigue crack into the inner core) and stage III (overall fracture), among which stage II occurs in the late stage beyond 85 to 90% of the fatigue life; at intermediate maximum stress, many large cracks grow into the core portion at different cross sections but not at high and low maximum stresses; accordingly, the critical current and residual strength of the portion apart from the main crack are low for the intermediate maximum stress but not for low and high maximum stresses.

  18. Assessment of average exposure to organochlorine pesticides in southern Togo from water, maize (Zea mays) and cowpea (Vigna unguiculata).

    PubMed

    Mawussi, G; Sanda, K; Merlina, G; Pinelli, E

    2009-03-01

    Drinking water, cowpea and maize grains were sampled in some potentially exposed agro-ecological areas in Togo and analysed for their contamination by some common organochlorine pesticides. A total of 19 organochlorine pesticides were investigated in ten subsamples of maize, ten subsamples of cowpea and nine subsamples of drinking water. Analytical methods included solvent extraction of the pesticide residues and their subsequent quantification using gas chromatography-mass spectrometry (GC/MS). Estimated daily intakes (EDIs) of pesticides were also determined. Pesticides residues in drinking water (0.04-0.40 microg l(-1)) were higher than the maximum residue limit (MRL) (0.03 microg l(-1)) set by the World Health Organization (WHO). Dieldrin, endrin, heptachlor epoxide and endosulfan levels (13.16-98.79 microg kg(-1)) in cowpea grains exceeded MRLs applied in France (10-50 microg kg(-1)). Contaminants' levels in maize grains (0.53-65.70 microg kg(-1)) were below the MRLs (20-100 microg kg(-1)) set by the Food and Agriculture Organization (FAO) and the WHO. EDIs of the tested pesticides ranged from 0.02% to 162.07% of the acceptable daily intakes (ADIs). Population exposure levels of dieldrin and heptachlor epoxide were higher than the FAO/WHO standards. A comprehensive national monitoring programme on organochlorine pesticides should be undertaken to include such other relevant sources like meat, fish, eggs and milk.

  19. Exposure assessment of chemical hazards in pork meat, liver, and kidney, and health impact implication in Hung Yen and Nghe An provinces, Vietnam.

    PubMed

    Tuyet-Hanh, Tran Thi; Sinh, Dang Xuan; Phuc, Pham Duc; Ngan, Tran Thi; Van Tuat, Chu; Grace, Delia; Unger, Fred; Nguyen-Viet, Hung

    2017-02-01

    This study assesses the risk of exposure to hazardous chemical residues in pork meat, liver, and kidney collected at wet markets in Nghe An and Hung Yen provinces and discusses health impact implication. 514 pig feed, kidney, liver, and pork samples were pooled and qualitatively and quantitatively analyzed for tetracyclines, fluoroquinolones, sulphonamide, chloramphenicol, β-agonists, and heavy metals. We compare the results with current regulations on chemical residues and discuss health implications. Legal antibiotics were found in feed. Tetracycline and fluoroquinolones were not present in pork, but 11% samples were positive with sulfamethazine above maximum residue limits (MRL); 11% of packaged feed and 4% of pork pooled samples were positive for chloramphenicol, a banned substance; two feed, two liver, and one pork samples were positive for β-agonists but did not exceed current MRL; 28% of pooled samples had lead, but all were below MRL; and all samples were negative for cadmium and arsenic. Thus, the health risks due to chemical hazards in pork in Hung Yen and Nghe An seemed not as serious as what were recently communicated to the public on the mass media. There is potential exposure to sulphonamide, chloramphenicol, and β-agonists from pork. Risk communication needs to focus on banned chemicals, while informing the public about the minimal risks associated with heavy metals.

  20. Voluntary Control of Residual Antagonistic Muscles in Transtibial Amputees: Feedforward Ballistic Contractions and Implications for Direct Neural Control of Powered Lower Limb Prostheses.

    PubMed

    Huang, Stephanie; Huang, He

    2018-04-01

    Discrete, rapid (i.e., ballistic like) muscle activation patterns have been observed in ankle muscles (i.e., plantar flexors and dorsiflexors) of able-bodied individuals during voluntary posture control. This observation motivated us to investigate whether transtibial amputees are capable of generating such a ballistic-like activation pattern accurately using their residual ankle muscles in order to assess whether the volitional postural control of a powered ankle prosthesis using proportional myoelectric control via residual muscles could be feasible. In this paper, we asked ten transtibial amputees to generate ballistic-like activation patterns using their residual lateral gastrocnemius and residual tibialis anterior to control a computer cursor via proportional myoelectric control to hit targets positioned at 20% and 40% of maximum voluntary contraction of the corresponding residual muscle. During practice conditions, we asked amputees to hit a single target repeatedly. During testing conditions, we asked amputees to hit a random sequence of targets. We compared movement time to target and end-point accuracy. We also examined motor recruitment synchronization via time-frequency representations of residual muscle activation. The result showed that median end-point error ranged from -0.6% to 1% maximum voluntary contraction across subjects during practice, which was significantly lower compared to testing ( ). Average movement time for all amputees was 242 ms during practice and 272 ms during testing. Motor recruitment synchronization varied across subjects, and amputees with the highest synchronization achieved the fastest movement times. End-point accuracy was independent of movement time. Results suggest that it is feasible for transtibial amputees to generate ballistic control signals using their residual muscles. Future work on volitional control of powered power ankle prostheses might consider anticipatory postural control based on ballistic-like residual muscle activation patterns and direct continuous proportional myoelectric control.

  1. Combined micromechanical and fabrication process optimization for metal-matrix composites

    NASA Technical Reports Server (NTRS)

    Morel, M.; Saravanos, D. A.; Chamis, C. C.

    1991-01-01

    A method is presented to minimize the residual matrix stresses in metal matrix composites. Fabrication parameters such as temperature and consolidation pressure are optimized concurrently with the characteristics (i.e., modulus, coefficient of thermal expansion, strength, and interphase thickness) of a fiber-matrix interphase. By including the interphase properties in the fabrication process, lower residual stresses are achievable. Results for an ultra-high modulus graphite (P100)/copper composite show a reduction of 21 percent for the maximum matrix microstress when optimizing the fabrication process alone. Concurrent optimization of the fabrication process and interphase properties show a 41 percent decrease in the maximum microstress. Therefore, this optimization method demonstrates the capability of reducing residual microstresses by altering the temperature and consolidation pressure histories and tailoring the interphase properties for an improved composite material. In addition, the results indicate that the consolidation pressures are the most important fabrication parameters, and the coefficient of thermal expansion is the most critical interphase property.

  2. Concurrent micromechanical tailoring and fabrication process optimization for metal-matrix composites

    NASA Technical Reports Server (NTRS)

    Morel, M.; Saravanos, D. A.; Chamis, Christos C.

    1990-01-01

    A method is presented to minimize the residual matrix stresses in metal matrix composites. Fabrication parameters such as temperature and consolidation pressure are optimized concurrently with the characteristics (i.e., modulus, coefficient of thermal expansion, strength, and interphase thickness) of a fiber-matrix interphase. By including the interphase properties in the fabrication process, lower residual stresses are achievable. Results for an ultra-high modulus graphite (P100)/copper composite show a reduction of 21 percent for the maximum matrix microstress when optimizing the fabrication process alone. Concurrent optimization of the fabrication process and interphase properties show a 41 percent decrease in the maximum microstress. Therefore, this optimization method demonstrates the capability of reducing residual microstresses by altering the temperature and consolidation pressure histories and tailoring the interphase properties for an improved composite material. In addition, the results indicate that the consolidation pressures are the most important fabrication parameters, and the coefficient of thermal expansion is the most critical interphase property.

  3. Residual Stress Distribution and Microstructure of a Multiple Laser-Peened Near-Alpha Titanium Alloy

    NASA Astrophysics Data System (ADS)

    Umapathi, A.; Swaroop, S.

    2018-04-01

    Laser peening without coating (LPwC) was performed on a Ti-2.5 Cu alloy with multiple passes (1, 3 and 5), using a Nd:YAG laser (1064 nm) at a constant overlap rate of 70% and power density of 6.7 GW cm-2. Hardness and residual stress profiles indicated thermal softening near the surface (< 100 μm) and bulk softening due to adiabatic heating. Maximum hardness (235 HV at 500 μm) and maximum residual stress (- 890 MPa at 100 μm) were observed for LPwC with 1 pass. Surface roughness and surface 3-D topography imaging showed that the surface roughness increased with the increase in the number of passes. XRD results indicated no significant β phases. However, peak shifts, broadening and asymmetry were observed and interpreted based on dislocation activity. Microstructures indicated no melting or resolidification or refinement of grains at the surface. Twin density was found to increase with the increase in the number of passes.

  4. Dissipation kinetics and safety evaluation of tebuconazole and trifloxystrobin in tea under tropical field conditions.

    PubMed

    Paramasivam, Mariappan; Deepa, Manthirachalam; Selvi, Chellamuthu; Chandrasekaran, Subramanian

    2017-12-01

    Dissipation kinetics of tebuconazole, trifloxystrobin and its acid metabolite residues were studied in tea under tropical field conditions using GC-MS (SIM). The average recoveries ranged from 80.7% to 105.8%, with a RSD of <9.3%. Dissipation rate for both doses applied followed first-order kinetics, with half-lives in green leaves in the range of 2.8-3.3 and 2.9-3.3 days; ranges in processed tea were 2.7-3.6 days for trifloxystrobin and 3.0-3.1 days for tebuconazole. The trifloxystrobin residues were not transferred into the tea infusion during the infusion process; tebuconazole did transfer, in the range of 14.3-18.9%. As the theoretical maximum residue contributions on tea from initial deposits were found to be less than the maximum permissible intake values, at the recommended application dose a withdrawal period of 23 days before consumption should be applied to reduce risk.

  5. Residual Stress Distribution and Microstructure of a Multiple Laser-Peened Near-Alpha Titanium Alloy

    NASA Astrophysics Data System (ADS)

    Umapathi, A.; Swaroop, S.

    2018-05-01

    Laser peening without coating (LPwC) was performed on a Ti-2.5 Cu alloy with multiple passes (1, 3 and 5), using a Nd:YAG laser (1064 nm) at a constant overlap rate of 70% and power density of 6.7 GW cm-2. Hardness and residual stress profiles indicated thermal softening near the surface (< 100 μm) and bulk softening due to adiabatic heating. Maximum hardness (235 HV at 500 μm) and maximum residual stress (- 890 MPa at 100 μm) were observed for LPwC with 1 pass. Surface roughness and surface 3-D topography imaging showed that the surface roughness increased with the increase in the number of passes. XRD results indicated no significant β phases. However, peak shifts, broadening and asymmetry were observed and interpreted based on dislocation activity. Microstructures indicated no melting or resolidification or refinement of grains at the surface. Twin density was found to increase with the increase in the number of passes.

  6. Organochlorine insecticide residues in soil and earthworms in the Delhi area, India, August-October 1974

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Yadav, D.V.; Mittal, P.K.; Agarwal, H.C.

    1981-09-01

    DDT residues in soil and earthworms from 50 sites in Delhi were monitored. DDT was detected in all but two samples each of soil and earthworms. Among DDT residues, p,p'-DDE was most common and was found in 48 samples each of soil and earthworms; p,p'-DDT was detected in only 43 soil samples and 46 earthworm samples. p,p'-TDE and o,p'-DDT were also present in smaller concentrations in 29 and 15 soil samples and in 43 and 25 earthworm samples, respectively. Maximum total DDT concentration of 2.6 ppm was detected in the soil from Durga Nagar in the vicinity of a DDTmore » factory. The highest concentration of 37.7 ppm total DDT in earthworms was also obtained from the same site. The maximum concentration factor found in the earthworms was 551. The total DDT concentration in the earthworms and soil showed significant correlation.« less

  7. Growing vegetables in developing countries for local urban populations and export markets: problems confronting small-scale producers.

    PubMed

    Dinham, Barbara

    2003-05-01

    Vegetables attract high applications of pesticides, and farmers in developing countries use many acutely toxic insecticides to control pests on these crops. With the liberalisation of agricultural markets in developing countries, the number of small-scale farmers growing vegetables for both domestic and export markets is increasing. Demand for supplies of year-round and exotic fruit and vegetables has grown in industrialised countries, but with rising quality standards and traceability requirements it is difficult for small-scale farmers to benefit from this lucrative non-traditional agricultural export trade. The demand is high for vegetables in the expanding cities in developing countries, and farmers in peri-urban areas, or rural areas with good access to the cities, are in a position to find a growing market for their produce. Poor storage facilities will often mean that farmers are forced to sell at peak times when prices are low. Farmers rarely have access to training in pesticide use, and have only limited or no access to advice on the complicated management of pesticides. The Food and Agriculture Organisation of the UN is concerned about high levels of poor quality and adulterated pesticides on sale in developing countries. Surveys repeatedly show that without training, farmers are unable to make good crop decisions: recognition of pests and their predators is generally low, leading to decisions to spray to kill any insect; knowledge of product selection, application rates and timing is poor; different products are often combined in the belief that the effect will be greater; re-entry periods after spraying and essential harvest intervals are not known; and without knowledge of alternatives, farmers will often assume that the only solution to pest problems is to spray more frequently. From a consumer's point of view, few developing countries are able to monitor pesticide residues, particularly for produce grown for home consumption: most countries do not have laboratories for even simple residue testing. Changes in European Maximum Residue Limits means that export crops will be rejected if they contain residues at the Limit of Detection of pesticides not registered in Europe. Season-long field level training in Integrated Pest Management can help farmers to become better decision-makers, and to greatly reduce pesticide use while reducing risks to their own health and environment, producing safer products for consumers, maintaining yields, and increasing incomes.

  8. Liquid chromatography-tandem mass spectrometry multiresidue method for the analysis of quaternary ammonium compounds in cheese and milk products: Development and validation using the total error approach.

    PubMed

    Slimani, Kahina; Féret, Aurélie; Pirotais, Yvette; Maris, Pierre; Abjean, Jean-Pierre; Hurtaud-Pessel, Dominique

    2017-09-29

    Quaternary ammonium compounds (QACs) are both cationic surfactants and biocidal substances widely used as disinfectants in the food industry. A sensitive and reliable method for the analysis of benzalkonium chlorides (BACs) and dialkyldimethylammonium chlorides (DDACs) has been developed that enables the simultaneous quantitative determination of ten quaternary ammonium residues in dairy products below the provisional maximum residue level (MRL), set at 0.1mgkg -1 . To the best of our knowledge, this method could be the one applicable to milk and to three major processed milk products selected, namely processed or hard pressed cheeses, and whole milk powder. The method comprises solvent extraction using a mixture of acetonitrile and ethyl acetate, without any further clean-up. Analyses were performed by liquid chromatography coupled with electrospray tandem mass spectrometry detection (LC-ESI-MS/MS) operating in positive mode. A C18 analytical column was used for chromatographic separation, with a mobile phase composed of acetonitrile and water both containing 0.3% formic acid; and methanol in the gradient mode. Five deuterated internal standards were added to obtain the most accurate quantification. Extraction recoveries were satisfactory and no matrix effects were observed. The method was validated using the total error approach in accordance with the NF V03-110 standard in order to characterize the trueness, repeatability, intermediate precision and analytical limits within the range of 5-150μgkg -1 for all matrices. These performance criteria, calculated by e.noval ® 3.0 software, were satisfactory and in full accordance with the proposed provisional MRL and with the recommendations in the European Union SANTE/11945/2015 regulatory guidelines. The limit of detection (LOD) was low (<1.9μgkg -1 ) and the limit of quantification (LOQ) ranged from 5μgkg -1 to 35μgkg -1 for all matrices depending on the analytes. The validation results proved that the method is suitable for quantifying quaternary ammoniums in foodstuffs from dairy industries at residue levels, and could be used for biocide residues monitoring plans and to measure the exposition consumer to biocides products. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Quantitative analysis of amoxicillin, its major metabolites and ampicillin in eggs by liquid chromatography combined with electrospray ionization tandem mass spectrometry.

    PubMed

    Sun, Lirui; Jia, Longfei; Xie, Xing; Xie, Kaizhou; Wang, Jianfeng; Liu, Jianyu; Cui, Lulu; Zhang, Genxi; Dai, Guojun; Wang, Jinyu

    2016-02-01

    In this present study, we developed a simple, rapid and specific method for the quantitative analysis of the contents of amoxicillin (AMO), AMO metabolites and ampicillin (AMP) in eggs. This method uses a simple liquid-liquid extraction with acetonitrile followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The optimized method has been validated according to requirements defined by the European Union and Food and Drug Administration. Extraction recoveries of the target compounds from the egg at 5, 10 and 25 μg/kg were all higher than 80%, with relative standard deviations not exceeding 10.00%. The limits of quantification in eggs were below the maximum residue limits (MRLs). The decision limits (CCα) ranged between 11.1 and 11.5 μg/kg, while detection capabilities (CCβ) from 12.1 to 13.0 μg/kg. These values were very close to the corresponding MRLs. Finally, the new approach was successfully verified for the quantitative determination of these analytes in 40 commercial eggs from local supermarkets. Copyright © 2015 Elsevier Ltd. All rights reserved.

  10. Metabolism and Residues of 2,4-Dichlorophenoxyacetic Acid in DAS-40278-9 Maize (Zea mays) Transformed with Aryloxyalkanoate Dioxygenase-1 Gene.

    PubMed

    Zhou, Xiao; Rotondaro, Sandra L; Ma, Mingming; Rosser, Steve W; Olberding, Ed L; Wendelburg, Brian M; Adelfinskaya, Yelena A; Balcer, Jesse L; Blewett, T Craig; Clements, Bruce

    2016-10-12

    DAS-40278-9 maize, which is developed by Dow AgroSciences, has been genetically modified to express the aryloxyalkanoate dioxygenase-1 (AAD-1) protein and is tolerant to phenoxy auxin herbicides, such as 2,4-dichlorophenoxyacetic acid (2,4-D). To understand the metabolic route and residue distribution of 2,4-D in DAS-40278-9 maize, a metabolism study was conducted with 14 C-radiolabeled 2,4-D applied at the maximum seasonal rate. Plants were grown in boxes outdoors. Forage and mature grain, cobs, and stover were collected for analysis. The metabolism study showed that 2,4-D was metabolized to 2,4-dichlorophenol (2,4-DCP), which was then rapidly conjugated with glucose. Field-scale residue studies with 2,4-D applied at the maximum seasonal rate were conducted at 25 sites in the U.S. and Canada to measure the residues of 2,4-D and free and conjugated 2,4-DCP in mature forage, grain, and stover. Residues of 2,4-D were not detectable in the majority of the grain samples and averaged <1.0 and <1.5 μg/g in forage and stover, respectively. Free plus conjugated 2,4-DCP was not observed in grain and averaged <1.0 μg/g in forage and stover.

  11. Ingestive Behavior of Ovine Fed with Marandu Grass Silage Added with Naturally Dehydrated Brewery Residue

    PubMed Central

    Lima de Souza, Alexandre; Divino Ribeiro, Marinaldo; Mattos Negrão, Fagton; Castro, Wanderson José Rodrigues; Valério Geron, Luiz Juliano; de Azevedo Câmara, Larissa Rodrigues

    2016-01-01

    The objective was to evaluate the ingestive behavior of ovine fed Marandu grass silage with dehydrated brewery residue added. The experiment had a completely randomized design with five treatments and four repetitions, with the treatments levels of inclusion being of 0, 10, 20, 30, and 40% natural matter of naturally dehydrated brewery residue for 36 hours to the marandu grass silage. 20 ovines were used and the experimental period was 21 days, 15 being for adaptation to diets. The use of brewery byproduct promoted quadratic effect (P < 0.05) for the consumption of dry matter with maximum point value estimated at adding 23.25% additive. Ingestion efficiency and rumination efficiency of dry matter (g DM/hour) were significant (P < 0.05), by quadratic behavior, and NDF ingestion and rumination efficiency showed crescent linear behavior. The DM and NDF consumption expressed in kg/meal and in minutes/kg were also significant (P < 0.05), showing quadratic behavior. Rumination activity expressed in g DM and NDF/piece was influenced (P < 0.05) by the adding of brewery residue in marandu grass silage in quadratic way, with maximum value estimated of 1.57 g DM/bolus chewed in inclusion of 24.72% additive in grass silage. The conclusion is that intermediary levels adding of 20 to 25% dehydrated brewery residue affects certain parameters of ingestive behavior. PMID:27547811

  12. Residues of azoxystrobin from grapes to raisins.

    PubMed

    Lentza-Rizos, Chaido; Avramides, Elizabeth J; Kokkinaki, Kalliopi

    2006-01-11

    Azoxystrobin, a fungicide of the strobilurin group, has an European Union maximum residue level (MRL) of 2 mg/kg for grapes. This work aimed to assess residues on fresh and washed grapes and on raisins following processing with (i) alkali treatment and sun drying and (ii) sun drying only. QUADRIS 25% SC was applied according to good agricultural practice for two consecutive years on a typical cv. Thomson seedless and a seed-producing clone. Samples were collected 0, 15, and 21 days postapplication and analyzed using gas chromatography/electron capture detection; recoveries were 86 +/- 12% for grapes and 99 +/- 15% for raisins. Residues on grapes were 0.49-1.84 mg/kg, and washing removed 75% of the residue. Residues in raisins produced from seedless grapes were 0.51-1.49 (treatment 1) and 1.42-2.08 mg/kg (treatment 2), with residue transfer factors sometimes >1, even following alkali treatment, which reduced residues considerably. To avoid trade problems, a higher MRL for raisins is necessary.

  13. 31 CFR 149.3 - Maximum obligation limitation.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 31 Money and Finance: Treasury 1 2014-07-01 2014-07-01 false Maximum obligation limitation. 149.3 Section 149.3 Money and Finance: Treasury Regulations Relating to Money and Finance MONETARY OFFICES, DEPARTMENT OF THE TREASURY CALCULATION OF MAXIMUM OBLIGATION LIMITATION § 149.3 Maximum obligation limitation...

  14. 24 CFR 232.903 - Maximum mortgage limitations.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 24 Housing and Urban Development 2 2010-04-01 2010-04-01 false Maximum mortgage limitations. 232... ASSISTED LIVING FACILITIES Insurance of Mortgages Covering Existing Projects § 232.903 Maximum mortgage limitations. Notwithstanding the maximum mortgage limitations set forth in § 232.30, a mortgage within the...

  15. 5 CFR 582.402 - Maximum garnishment limitations.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 5 Administrative Personnel 1 2010-01-01 2010-01-01 false Maximum garnishment limitations. 582.402... Maximum garnishment limitations. Pursuant to section 1673(a)(1) of title 15 of the United States Code (the... Federal Regulations, part 870, the following limitations are applicable: (a) Unless a lower maximum...

  16. 5 CFR 581.402 - Maximum garnishment limitations.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 5 Administrative Personnel 1 2010-01-01 2010-01-01 false Maximum garnishment limitations. 581.402... § 581.402 Maximum garnishment limitations. (a) Except as provided in paragraph (b) of this section... Protection Act, as amended), unless a lower maximum garnishment limitation is provided by applicable State or...

  17. Twyman effect mechanics in grinding and microgrinding.

    PubMed

    Lambropoulos, J C; Xu, S; Fang, T; Golini, D

    1996-10-01

    In the Twyman effect (1905), when one side of a thin plate with both sides polished is ground, the plate bends: The ground side becomes convex and is in a state of compressive residual stress, described in terms of force per unit length (Newtons per meter) induced by grinding, the stress (Newtons per square meter) induced by grinding, and the depth of the compressive layer (micrometers). We describe and correlate experiments on optical glasses from the literature in conditions of loose abrasive grinding (lapping at fixed nominal pressure, with abrasives 4-400 μm in size) and deterministic microgrinding experiments (at a fixed infeed rate) conducted at the Center for Optics Manufacturing with bound diamond abrasive tools (with a diamond size of 3-40 μm, embedded in metallic bond) and loose abrasive microgrinding (abrasives of less than 3 μm in size). In brittle grinding conditions, the grinding force and the depth of the compressive layer correlate well with glass mechanical properties describing the fracture process, such as indentation crack size. The maximum surface residual compressive stress decreases, and the depth of the compressive layer increases with increasing abrasive size. In lapping conditions the depth of the abrasive grain penetration into the glass surface scales with the surface roughness, and both are determined primarily by glass hardness and secondarily by Young's modulus for various abrasive sizes and coolants. In the limit of small abrasive size (ductile-mode grinding), the maximum surface compressive stress achieved is near the yield stress of the glass, in agreement with finite-element simulations of indentation in elastic-plastic solids.

  18. Comparison of Insecticide Susceptibilities of Empoasca vitis (Hemiptera: Cicadellidae) from Three Main Tea-Growing Regions in China.

    PubMed

    Wei, Qi; Yu, Hua-Yang; Niu, Chun-Dong; Yao, Rong; Wu, Shun-Fan; Chen, Zhuo; Gao, Cong-Fen

    2015-06-01

    Empoasca vitis (Göthe) is an important insect pest in tea-growing areas of China, and chemical control is the main tactic for the management of this pest. Due to the pressure of increasing insecticide resistance and more stringent food safety regulations, development of sound IPM strategies for E. vitis is an urgent matter. This study comparatively evaluated four field populations of E. vitis from three different tea-growing regions in China for their susceptibilities to eight insecticides using a simple leaf-dip methodology. E. vitis was found to be most sensitive to indoxacarb (LC50<0.5 mg/liter) and least sensitive to isoprocarb (LC50>5 mg/liter) and sophocarpidine (LC50>95 mg/liter, a botanical pesticide) regardless of populations. Population (geographical) variations were higher for indoxacarb and imidacloprid than other compounds. Judging by the 95% fiducial limits of LC50 values, all populations had similar susceptibilities to chlorfenapyr, bifenthrin, and acetamiprid or imidacloprid. Correlation analysis suggested that chlorfenapyr and indoxacarb or isoprocarb may have a high risk of cross resistance. Considering potency (LC50) and maximum residual levels, chlorfenapyr and bifenthrin are good insecticide options followed by acetamiprid and indoxacarb. These results provide valuable information to intelligently select insecticides for IPM programs that are efficacious against E. vitis while also managing insecticide resistance and maximum residual levels for tea production in China. © The Authors 2015. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  19. 5 CFR 550.105 - Biweekly maximum earnings limitation.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 5 Administrative Personnel 1 2010-01-01 2010-01-01 false Biweekly maximum earnings limitation. 550... PAY ADMINISTRATION (GENERAL) Premium Pay Maximum Earnings Limitations § 550.105 Biweekly maximum... basic pay and premium pay for any biweekly pay period to exceed the greater of— (1) The maximum biweekly...

  20. 5 CFR 550.106 - Annual maximum earnings limitation.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 5 Administrative Personnel 1 2010-01-01 2010-01-01 false Annual maximum earnings limitation. 550... PAY ADMINISTRATION (GENERAL) Premium Pay Maximum Earnings Limitations § 550.106 Annual maximum... and premium pay for the calendar year to exceed the greater of— (1) The maximum annual rate of basic...

  1. Energy performance of an integrated bio-and-thermal hybrid system for lignocellulosic biomass waste treatment.

    PubMed

    Kan, Xiang; Yao, Zhiyi; Zhang, Jingxin; Tong, Yen Wah; Yang, Wenming; Dai, Yanjun; Wang, Chi-Hwa

    2017-03-01

    Lignocellulosic biomass waste, a heterogeneous complex of biodegradables and non-biodegradables, accounts for large proportion of municipal solid waste. Due to limitation of single-stage treatment, a two-stage hybrid AD-gasification system was proposed in this work, in which AD acted as pre-treatment to convert biodegradables into biogas followed by gasification converting solid residue into syngas. Energy performance of single and two-stage systems treating 3 typical lignocellulosic wastes was studied using both experimental and numerical methods. In comparison with conventional single-stage gasification treatment, this hybrid system could significantly improve the quality of produced gas for all selected biomass wastes and show its potential in enhancing total gas energy production by a maximum value of 27% for brewer's spent grain treatment at an organic loading rate (OLR) of 3gVS/L/day. The maximum overall efficiency of the hybrid system for horticultural waste treatment was 75.2% at OLR of 11.3gVS/L/day, 5.5% higher than conventional single-stage system. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Bioprosthetic Valve Fracture During Valve-in-valve TAVR: Bench to Bedside.

    PubMed

    Saxon, John T; Allen, Keith B; Cohen, David J; Chhatriwalla, Adnan K

    2018-01-01

    Valve-in-valve (VIV) transcatheter aortic valve replacement (TAVR) has been established as a safe and effective means of treating failed surgical bioprosthetic valves (BPVs) in patients at high risk for complications related to reoperation. Patients who undergo VIV TAVR are at risk of patient-prosthesis mismatch, as the transcatheter heart valve (THV) is implanted within the ring of the existing BPV, limiting full expansion and reducing the maximum achievable effective orifice area of the THV. Importantly, patient-prosthesis mismatch and high residual transvalvular gradients are associated with reduced survival following VIV TAVR. Bioprosthetic valve fracture (BVF) is as a novel technique to address this problem. During BPV, a non-compliant valvuloplasty balloon is positioned within the BPV frame, and a highpressure balloon inflation is performed to fracture the surgical sewing ring of the BPV. This allows for further expansion of the BPV as well as the implanted THV, thus increasing the maximum effective orifice area that can be achieved after VIV TAVR. This review focuses on the current evidence base for BVF to facilitate VIV TAVR, including initial bench testing, procedural technique, clinical experience and future directions.

  3. Acid hydrolysis of Curcuma longa residue for ethanol and lactic acid fermentation.

    PubMed

    Nguyen, Cuong Mai; Nguyen, Thanh Ngoc; Choi, Gyung Ja; Choi, Yong Ho; Jang, Kyoung Soo; Park, Youn-Je; Kim, Jin-Cheol

    2014-01-01

    This research examines the acid hydrolysis of Curcuma longa waste, to obtain the hydrolysate containing lactic acid and ethanol fermentative sugars. A central composite design for describing regression equations of variables was used. The selected optimum condition was 4.91% sulphuric acid, 122.68°C and 50 min using the desirability function under the following conditions: the maximum reducing sugar (RS) yield is within the limited range of the 5-hydroxymethylfurfural (HMF) and furfural concentrations. Under the condition, the obtained solution contained 144 g RS/L, 0.79 g furfural/L and 2.59 g HMF/L and was directly fermented without a detoxification step. The maximum product concentration, average productivity, RS conversion and product yield were 115.36 g/L, 2.88 g/L/h, 89.43% and 64% for L-lactic acid; 113.92 g/L, 2.59 g/L/h, 88.31% and 63.29% for D-lactic acid; and 55.03 g/L, 1.38 g/L/h, 42.66 and 30.57%, respectively, for ethanol using a 7-L jar fermenter. Copyright © 2013. Published by Elsevier Ltd.

  4. Detection of quinolones in commercial eggs obtained from farms in the Espaíllat Province in the Dominican Republic.

    PubMed

    Moscoso, S; de los Santos, F Solís; Andino, A G; Diaz-Sanchez, Sandra; Hanning, I

    2015-01-01

    Previously, we reported the use of quinolones in broiler chickens resulted in residues in retail poultry meat obtained from nine districts in the Santiago Province of the Dominican Republic. Residues in poultry products are a concern due to consumer allergies and the potential to develop antibiotic-resistant bacteria. Given the use of quinolones in poultry production and our previous findings in poultry meat, the objective of this study was to evaluate the presence of quinolone residues in eggs. Samples were collected from 48 different farms located in three of the four municipalities (Moca, Cayetano Germosén, and Jamao) of the Espaíllat Province. Each farm was sampled three times between July and September for a total of 144 samples. Samples were evaluated qualitatively and quantitatively for quinolone residues using the Equinox test. Operation systems (cage or floor), seasonality, and location were considered along with egg-producer sizes that were defined as small scale, <30,000 eggs per day; medium scale, 30,000 to 60,000 eggs per day; or large scale, >60,000 eggs per day. From small-, medium-, and large-scale producers, 69, 50, and 40% of samples were positive for quinolone residues, respectively. A greater number of samples were positive (61%) in floor-laying hen producers compared with those using cages (40%). In the Jamao municipality, 67% of the samples were positive compared with Moca and Cayetano Germosén, where 56 and 25% of samples were positive, respectively. Sampling time had an effect on percent positives: samples collected in July, August, and September were 71, 19, and 63% positive, respectively. Overall, 51% of the samples obtained from eggs produced in the province of Espaíllat were positive for quinolone residues at levels higher than the maximum limits for edible tissue established by the regulatory agencies, including the European Union and U.S. Department of Agriculture. The results obtained from this research confirmed the presence of quinolone residue in eggs, which may present a health risk to some consumers.

  5. A study on experimental characteristic of microwave-assisted pyrolysis of microalgae.

    PubMed

    Hu, Zhifeng; Ma, Xiaoqian; Chen, Chunxiang

    2012-03-01

    The microwave-assisted pyrolysis of Chlorella vulgaris was carried out under different microwave power levels, catalysts and contents of activated carbon and solid residue. The products, pyrolysis temperature and temperature rising rate were analyzed in order to obtain the optimal conditions. The results indicated that the higher the microwave power level was, the higher the maximum temperature rising rate and pyrolysis temperature were. The maximum bio-oil yield (35.83 wt.%) and gas yield (52.37%) were achieved under the microwave power of 1500 W and 2250 W, respectively. And 2250 W was the optimal power to obtain bio-fuel product. High microwave power level and catalyst can enhance the production of gas. Catalysts can promote the pyrolysis of C. vulgaris, and activated carbon was the best among the tested catalysts followed by the solid residue. The optimal content of activated carbon is 5% with the maximum bio-fuel yield of 87.47%. Copyright © 2011 Elsevier Ltd. All rights reserved.

  6. A novel inhibition based biosensor using urease nanoconjugate entrapped biocomposite membrane for potentiometric glyphosate detection.

    PubMed

    Vaghela, Chetana; Kulkarni, Mohan; Haram, Santosh; Aiyer, Rohini; Karve, Meena

    2018-03-01

    A potentiometric biosensor based on agarose-guar gum (A-G) entrapped bio-nanoconjugate of urease with gold nanoparticles (AUNps), has been reported for the first time for glyphosate detection. The biosensor is based on inhibition of urease activity by glyphosate, which was measured by direct potentiometry using ammonium ion selective electrode covered with A-G-urease nanoconjugate membrane. TEM and FTIR analysis revealed nanoconjugate formation and its immobilization in A-G matrix respectively. The composite biopolymer employed for immobilization yields thin, transparent, flexible membrane having superior mechanical strength and stability. It retains the maximum activity (92%) of urease with negligible leaching. The conjugation of urease with AUNps allows improvement in response characteristics for potentiometric measurement. The biosensor shows a linear response in the glyphosate concentration range from 0.5ppm-50ppm, with limit of detection at 0.5ppm, which covers maximum residual limit set by WHO for drinking water. The inhibition of catalytic activity of urease nanoconjugate by gyphosate was confirmed by FTIR analysis. The response of fabricated biosensor is selective towards glyphosate as against various other pesticides. The biosensor exhibits good performance in terms of reproducibility and prolonged storage stability of 180days. Thus, the present biosensor provides an alternative method for simple, selective and cost effective detection of glyphosate based on urease inhibition. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Total and inorganic arsenic in Iranian rice.

    PubMed

    Cano-Lamadrid, Marina; Munera-Picazo, Sandra; Burló, Francisco; Hojjati, Mohammad; Carbonell-Barrachina, Ángel A

    2015-05-01

    It is well known that arsenic (As) exposure, particularly to inorganic species (i-As), has adverse effects on humans. Nowadays, the European Union (EU) has still not regulated the maximum residue limit of As in commercial samples of rice and rice-based products, although it is actively working on the topic. The European Food Safety Authority (EFSA) is collecting data on total arsenic (t-As) and i-As from different rice-producing regions not only from EU countries but also from other parts of the world to finally set up this maximum threshold. As Iran is a rice-producing country, the aim of this work was to evaluate the contents of t-As and i-As in 15 samples of Iranian white, nonorganic, and aromatic rice collected from the most important rice-producing regions of the country. The means of t-As and i-As were 120 and 82 μg/kg, respectively. The experimental i-As mean in Iranian rice was below the Chinese standard for the i-As in rice, 150 μg/kg, and the Food and Agriculture Organization of the United Nations (FAO) limit, 200 μg/kg. Therefore, Iranian rice seems to have reasonable low i-As content and it is safe to be marketed in any market, including China and the EU. © 2015 Institute of Food Technologists®

  8. Production of surfactin from rice mill polishing residue by submerged fermentation using Bacillus subtilis MTCC 2423.

    PubMed

    Gurjar, Jigar; Sengupta, Bina

    2015-08-01

    Rice mill polishing residue (RMPR), an abundant and cheap agro residue, was used as substrate for microbial growth of Bacillus subtilis MTCC 2423 by submerged fermentation process to produce surfactin. Nutrients present in the residue were sufficient to sustain the growth of the microorganism. Multi stage foam fractionation followed by acid precipitation was used to concentrate and recover the product. Recoverable yield of surfactin was 4.17 g/kg residue. Product recovered in the foamate accounted for 69% of the total yield. The residual broth containing ∼ 30% surfactin exhibited biological oxygen demand and chemical oxygen demand values of 23 and 69 mg/L respectively. The microbial growth data was correlated using three parameter sigmoid models. Surfactin synthesized had a predominance of molecular weight 1076 Da. Foam separation of copper using surfactin resulted in a maximum removal of 72.5%. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. Effects of fatigue and environment on residual strengths of center-cracked graphite/epoxy buffer strip panels

    NASA Technical Reports Server (NTRS)

    Bigelow, Catherine A.

    1989-01-01

    The effects of fatigue, moisture conditioning, and heating on the residual tension strengths of center-cracked graphite/epoxy buffer strip panels were evaluated using specimens made with T300/5208 graphite epoxy in a 16-ply quasi-isotropic layup, with two different buffer strip materials, Kevlar-49 or S-glass. It was found that, for panels subjected to fatigue loading, the residual strengths were not significantly affected by the fatigue loading, the number of repetitions of the loading spectrum, or the maximum strain level. The moisture conditioning reduced the residual strengths of the S-glass buffer strip panels by 10 to 15 percent below the ambient results, but increased the residual strengths of the Kevlar-49 buffer strip panels slightly. For both buffer strip materials, the heat increased the residual strengths of the buffer strip panels slightly over the ambient results.

  10. Residues of azoxystrobin, fenhexamid and pyrimethanil in strawberry following field treatments and the effect of domestic washing.

    PubMed

    Angioni, A; Schirra, M; Garau, V L; Melis, M; Tuberoso, C I G; Cabras, P

    2004-11-01

    Residues of the pesticides azoxystrobin, fenhexamid and pyrimethanil were determined in strawberry after field treatment. The effect of 'home' washing with tap water and a commercially available vegetable detergent on residue levels was also studied. After treatment, azoxystrobin and pyrimethanil residues on strawberry were on average 0.55 and 2.98 mg kg(-1), respectively, values below the maximum residue level (MRL) fixed by the European Union (2.0 and 5 mg kg(-1), respectively), while fenhexamid residues were on average 2.99 mg kg(-1), which is very close to the MRL of 3.0 mg kg(-1), but some samples were over the MRL. Thereafter, all residues declined, with a half-life of about 8 days (azoxystrobin and fenhexamid) and 4.8 days (pyrimethanil). Washing the fruit with tap water reduced the residues of azoxystrobin and fenhexamid but did not affect pyrimethanil residues. Finally, when fruits were washed with a commercial detergent, greater amounts were removed (about 45% of azoxystrobin and pyrimethanil and 60% of fenhexamid).

  11. Effects of Fine Particle Peening Conditions on the Rotational Bending Fatigue Strength of a Vacuum-Carburized Transformation-Induced Plasticity-Aided Martensitic Steel

    NASA Astrophysics Data System (ADS)

    Sugimoto, Koh-ichi; Hojo, Tomohiko; Mizuno, Yuta

    2018-02-01

    The effects of fine particle peening conditions on the rotational bending fatigue strength of a vacuum-carburized transformation-induced plasticity-aided martensitic steel with a chemical composition of 0.20 pct C, 1.49 pct Si, 1.50 pct Mn, 0.99 pct Cr, 0.02 pct Mo, and 0.05 pct Nb were investigated for the fabrication of automotive drivetrain parts. The maximum fatigue limit, resulting from high hardness and compressive residual stress in the surface-hardened layer caused by the severe plastic deformation and the strain-induced martensite transformation of the retained austenite during fine particle peening, was obtained by fine particle peening at an arc height of 0.21 mm (N). The high fatigue limit was also a result of the increased martensite fraction and the active plastic relaxation via the strain-induced martensite transformation during fatigue deformation, as well as preferential crack initiation on the surface or at the subsurface.

  12. Quantitative determination of several synthetic corticosteroids by gas chromatography-mass spectrometry after purification by immunoaffinity chromatography.

    PubMed

    Delahaut, P; Jacquemin, P; Colemonts, Y; Dubois, M; De Graeve, J; Deluyker, H

    1997-08-29

    A study was conducted to test a multiresidue analytical procedure for detecting and quantifying several corticosteroids on which the European Union imposes maximum residue limits (MRLs). Primary extracts from different matrices (liver, milk, urine, faeces) were first purified on C18 cartridges. A new immunoaffinity clean-up step was included. The immunoaffinity gel was used to purify several corticosteroids simultaneously with enrichment of the corresponding fractions. The extracts were treated with an aqueous solution of pyridinium chlorochromate to fully oxidise all corticosteroids and to facilitate their extraction with dichloromethane. After evaporation, the final extract was reconstituted with toluene before injection into the GC-MS apparatus. The analysis was performed in the CI-negative ionisation mode using ammonia as the reactant gas. The estimated detection and quantification limits were, respectively, 0.25 and 0.5 ppb or lower. Overall, the method is reproducible to within 20%. Recovery is between 50 and 80% according to the corticosteroid.

  13. Micro-solid-phase extraction (µ-SPE) of organophosphorous pesticides from wheat followed by LC-MS/MS determination.

    PubMed

    Della Pelle, Flavio; Di Crescenzo, Maria Chiara; Sergi, Manuel; Montesano, Camilla; Di Ottavio, Francesca; Scarpone, Rossana; Scortichini, Giampiero; Compagnone, Dario

    2016-01-01

    A rapid, selective and effective method of extraction, clean-up and concentration of organophosphorous pesticides from wheat followed by electrospray (ESI) LC-MS/MS analysis was developed. The μ-SPE (micro-solid-phase extraction) procedure resulted in good analytical performance and reduced at the same time matrix effects, analysis time and solvent consumption. Limits of detection (LODs) and quantification (LOQs) were in the range of 0.3-10 and 1-30 μg kg(-1), respectively, with good reproducibility (RSD ≤ 13.8) and recoveries between 75% and 109%. Coefficients of determination (r(2)) were greater than 0.996 for the studied pesticides. Despite the reduced sorbent bed mass of μ-SPE tips (4.2 mg), the analytical data showed that no saturation phenomena occurs in the tested range of concentration both for single compounds and mixtures. Several real samples were analysed and the concentrations of the selected pesticides were found to be below the respective maximum residue limit (MRLs).

  14. Photon Counting Data Analysis: Application of the Maximum Likelihood and Related Methods for the Determination of Lifetimes in Mixtures of Rose Bengal and Rhodamine B

    DOE PAGES

    Santra, Kalyan; Smith, Emily A.; Petrich, Jacob W.; ...

    2016-12-12

    It is often convenient to know the minimum amount of data needed in order to obtain a result of desired accuracy and precision. It is a necessity in the case of subdiffraction-limited microscopies, such as stimulated emission depletion (STED) microscopy, owing to the limited sample volumes and the extreme sensitivity of the samples to photobleaching and photodamage. We present a detailed comparison of probability-based techniques (the maximum likelihood method and methods based on the binomial and the Poisson distributions) with residual minimization-based techniques for retrieving the fluorescence decay parameters for various two-fluorophore mixtures, as a function of the total numbermore » of photon counts, in time-correlated, single-photon counting experiments. The probability-based techniques proved to be the most robust (insensitive to initial values) in retrieving the target parameters and, in fact, performed equivalently to 2-3 significant figures. This is to be expected, as we demonstrate that the three methods are fundamentally related. Furthermore, methods based on the Poisson and binomial distributions have the desirable feature of providing a bin-by-bin analysis of a single fluorescence decay trace, which thus permits statistics to be acquired using only the one trace for not only the mean and median values of the fluorescence decay parameters but also for the associated standard deviations. Lastly, these probability-based methods lend themselves well to the analysis of the sparse data sets that are encountered in subdiffraction-limited microscopies.« less

  15. Elasto-limited plastic analysis of structures for probabilistic conditions

    NASA Astrophysics Data System (ADS)

    Movahedi Rad, M.

    2018-06-01

    With applying plastic analysis and design methods, significant saving in material can be obtained. However, as a result of this benefit excessive plastic deformations and large residual displacements might develop, which in turn might lead to unserviceability and collapse of the structure. In this study, for deterministic problem the residual deformation of structures is limited by considering a constraint on the complementary strain energy of the residual forces. For probabilistic problem the constraint for the complementary strain energy of the residual forces is given randomly and critical stresses updated during the iteration. Limit curves are presented for the plastic limit load factors. The results show that these constraints have significant effects on the load factors. The formulations of the deterministic and probabilistic problems lead to mathematical programming which are solved by the use of nonlinear algorithm.

  16. Axial residual stresses in boron fibers

    NASA Technical Reports Server (NTRS)

    Behrendt, D. R.

    1978-01-01

    The axial residual stress distribution as a function of radius was determined from the fiber surface to the core including the average residual stress in the core. Such measurements on boron on tungsten (B/W) fibers show that the residual stresses for 102, 142, 203, and 366 micron diameter fibers were similar, being compressive at the surface and changing monotonically to a region of tensile within the boron. At approximately 25 percent of the original radius, the stress reaches a maximum tensile stress of about 860 mn/sq.m and then decreases to a compressive stress near the tungsten boride core. Data were presented for 203 micron diameter B/W fibers that show annealing above 900 C reduces the residual stresses. A comparison between 102 micron diameter B/W and boron on carbon (b/C) shows that the residual stresses were similar in the outer regions of the fibers, but that large differences near and in the core were observed. The effects of these residual stresses on the fracture of boron fibers were discussed.

  17. Residue pattern of polycyclic aromatic hydrocarbons during green tea manufacturing and their transfer rates during tea brewing.

    PubMed

    Gao, Guanwei; Chen, Hongping; Liu, Pingxiang; Hao, Zhenxia; Ma, Guicen; Chai, Yunfeng; Wang, Chen; Lu, Chengyin

    2017-06-01

    Residues of polycyclic aromatic hydrocarbons (PAHs) in green tea and tea infusion were determined using gas chromatography-tandem mass spectrometry to study their dissipation pattern during green tea processing and infusion. Concentration and evaporation of PAHs during tea processing were the key factors affecting PAH residue content in product intermediates and in green tea. PAH residues in tea leaves increased by 2.4-3.1 times during the manufacture of green tea using the electric heating model. After correction to dry weight, PAH residue concentrations decreased by 33.5-48.4% during green tea processing because of PAH evaporation. Moreover, spreading and drying reduced PAH concentrations. The transfer rates of PAH residues from green tea to infusion varied from 4.6% to 7.2%, and PAH leaching was higher in the first infusion than in the second infusion. These results are useful for assessing exposure to PAHs from green tea and in formulating controls for the maximum residue level of PAHs in green tea.

  18. Effect of radiance-to-reflectance transformation and atmosphere removal on maximum likelihood classification accuracy of high-dimensional remote sensing data

    NASA Technical Reports Server (NTRS)

    Hoffbeck, Joseph P.; Landgrebe, David A.

    1994-01-01

    Many analysis algorithms for high-dimensional remote sensing data require that the remotely sensed radiance spectra be transformed to approximate reflectance to allow comparison with a library of laboratory reflectance spectra. In maximum likelihood classification, however, the remotely sensed spectra are compared to training samples, thus a transformation to reflectance may or may not be helpful. The effect of several radiance-to-reflectance transformations on maximum likelihood classification accuracy is investigated in this paper. We show that the empirical line approach, LOWTRAN7, flat-field correction, single spectrum method, and internal average reflectance are all non-singular affine transformations, and that non-singular affine transformations have no effect on discriminant analysis feature extraction and maximum likelihood classification accuracy. (An affine transformation is a linear transformation with an optional offset.) Since the Atmosphere Removal Program (ATREM) and the log residue method are not affine transformations, experiments with Airborne Visible/Infrared Imaging Spectrometer (AVIRIS) data were conducted to determine the effect of these transformations on maximum likelihood classification accuracy. The average classification accuracy of the data transformed by ATREM and the log residue method was slightly less than the accuracy of the original radiance data. Since the radiance-to-reflectance transformations allow direct comparison of remotely sensed spectra with laboratory reflectance spectra, they can be quite useful in labeling the training samples required by maximum likelihood classification, but these transformations have only a slight effect or no effect at all on discriminant analysis and maximum likelihood classification accuracy.

  19. Development and validation of modified QuEChERS method coupled with LC-MS/MS for simultaneous determination of cymiazole, fipronil, coumaphos, fluvalinate, amitraz, and its metabolite in various types of honey and royal jelly.

    PubMed

    Zheng, Weijia; Park, Jin-A; Abd El-Aty, A M; Kim, Seong-Kwan; Cho, Sang-Hyun; Choi, Jeong-Min; Yi, Hee; Cho, Soo-Min; Ramadan, Amer; Jeong, Ji Hoon; Shim, Jae-Han; Shin, Ho-Chul

    2018-01-01

    Over the past few decades, honey products have been polluted by different contaminants, such as pesticides, which are widely applied in agriculture. In this work, a modified EN - quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method was developed for the simultaneous quantification of pesticide residues, including cymiazole, fipronil, coumaphos, fluvalinate, amitraz, and its metabolite 2,4-dimethylaniline (2,4-DMA), in four types of honey (acacia, wild, chestnut, and manuka) and royal jelly. Samples were buffered with 0.2M dibasic sodium phosphate (pH 9), and subsequently, acetonitrile was employed as the extraction solvent. A combination of primary secondary amine (PSA) and C18 sorbents was used for purification prior to liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI + /MS-MS) analysis. The estimated linearity measured at six concentration levels presented good correlation coefficients (R 2 )≥0.99. The recovery, calculated from three different spiking levels, was 62.06-108.79% in honey and 67.58-106.34% in royal jelly, with an RSD<12% for all the tested compounds. The matrix effect was also evaluated, and most of the analytes presented signal enhancement. The limits of quantification (LOQ) ranged between 0.001 and 0.005mg/kg in various samples. These are considerably lower than the maximum residue limits (MRL) set by various regulatory authorities. A total of 43 market (domestic and imported) samples were assayed for method application. Among the tested samples, three samples were tested positive (i.e. detected and quantified) only for cymiazole residues. The residues in the rest of the samples were detected but not quantified. We concluded that the protocol developed in this work is simple and versatile for the routine quantification of cymiazole, 2,4-DMA, fipronil, coumaphos, amitraz, and fluvalinate in various types of honey and royal jelly. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Parametric models to compute tryptophan fluorescence wavelengths from classical protein simulations.

    PubMed

    Lopez, Alvaro J; Martínez, Leandro

    2018-02-26

    Fluorescence spectroscopy is an important method to study protein conformational dynamics and solvation structures. Tryptophan (Trp) residues are the most important and practical intrinsic probes for protein fluorescence due to the variability of their fluorescence wavelengths: Trp residues emit in wavelengths ranging from 308 to 360 nm depending on the local molecular environment. Fluorescence involves electronic transitions, thus its computational modeling is a challenging task. We show that it is possible to predict the wavelength of emission of a Trp residue from classical molecular dynamics simulations by computing the solvent-accessible surface area or the electrostatic interaction between the indole group and the rest of the system. Linear parametric models are obtained to predict the maximum emission wavelengths with standard errors of the order 5 nm. In a set of 19 proteins with emission wavelengths ranging from 308 to 352 nm, the best model predicts the maximum wavelength of emission with a standard error of 4.89 nm and a quadratic Pearson correlation coefficient of 0.81. These models can be used for the interpretation of fluorescence spectra of proteins with multiple Trp residues, or for which local Trp environmental variability exists and can be probed by classical molecular dynamics simulations. © 2018 Wiley Periodicals, Inc. © 2018 Wiley Periodicals, Inc.

  1. Skeletal maturation, fundamental motor skills and motor coordination in children 7-10 years.

    PubMed

    Freitas, Duarte L; Lausen, Berthold; Maia, José António; Lefevre, Johan; Gouveia, Élvio Rúbio; Thomis, Martine; Antunes, António Manuel; Claessens, Albrecht L; Beunen, Gaston; Malina, Robert M

    2015-01-01

    Relationships between skeletal maturation and fundamental motor skills and gross motor coordination were evaluated in 429 children (213 boys and 216 girls) 7-10 years. Skeletal age was assessed (Tanner-Whitehouse 2 method), and stature, body mass, motor coordination (Körperkoordinations Test für Kinder, KTK) and fundamental motor skills (Test of Gross Motor Development, TGMD-2) were measured. Relationships among chronological age, skeletal age (expressed as the standardised residual of skeletal age on chronological age) and body size and fundamental motor skills and motor coordination were analysed with hierarchical multiple regression. Standardised residual of skeletal age on chronological age interacting with stature and body mass explained a maximum of 7.0% of the variance in fundamental motor skills and motor coordination over that attributed to body size per se. Standardised residual of skeletal age on chronological age alone accounted for a maximum of 9.0% of variance in fundamental motor skills, and motor coordination over that attributed to body size per se and interactions between standardised residual of skeletal age on chronological age and body size. In conclusion, skeletal age alone or interacting with body size has a negligible influence on fundamental motor skills and motor coordination in children 7-10 years.

  2. Simultaneous determination and risk assessment of metalaxyl and azoxystrobin in potato by liquid chromatography with tandem mass spectrometry.

    PubMed

    Yu, Weiwei; Luo, Xiaoshuang; Qin, Xinxian; Huang, Min; Li, Jian; Zeng, Song; Zhang, Kankan; Hu, Deyu

    2018-05-09

    A liquid chromatography with tandem mass spectrometry method was developed and validated to simultaneously determine metalaxyl and azoxystrobin in soil, potato, and potato foliage samples. The samples were extracted by 20 mL of acetonitrile and purified with dispersive solid-phase extraction using octadecyl silane as sorbent. The method showed good linearity (determination coefficients ≥ 0.9926) for metalaxyl (2.5-500 ng/mL) and azoxystrobin (5-1000 ng/mL). The limits of detection and quantification for both fungicides were 1.5-20 μg/kg. The average recoveries in soil, potato, and potato foliage were 83.07-92.87% for metalaxyl and 82.71-98.53% for azoxystrobin. The intra- and inter-day relative standard deviations were all less than 9%. The method was successfully applied on the residual analysis of metalaxyl and azoxystrobin in field trial samples. The results showed that the concentrations of metalaxyl and azoxystrobin in potato samples collected from Guizhou and Hunan were below 50 and 100 μg/kg (maximum residue limit set by China), respectively, at 5 days after the last application. When following the recommended application manual, metalaxyl and azoxystrobin do not present health concerns to the population because the risk quotients are far below 100%. All the above data could help and promote the safe and proper use of metalaxyl and azoxystrobin in potato.

  3. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fritz, Brad G.; Dirkes, Roger L.; Napier, Bruce A.

    The Hanford Reach National Monument (HRNM) was created by presidential proclamation in 2000. It is located along the Columbia River in south central Washington and consists of five distinct units. The McGee Ranch-Riverlands and the North Slope units are addressed in this report. North Slope refers to two of the HRNM units: the Saddle Mountain Unit and the Wahluke Slope Unit. The Saddle Mountain and Wahluke Slope Units are located north of the Columbia River, while the McGee Ranch-Riverlands Unit is located south of the Columbia River and north and west of Washington State Highway 24. To fulfill internal U.S.more » Department of Energy (DOE) requirements prior to any radiological clearance of land, the DOE must evaluate the potential for residual radioactive contamination on this land and determine compliance with the requirements of DOE Order 5400.5. Authorized limits for residual radioactive contamination were developed based on the DOE annual exposure limit to the public (100 mrem) using future potential land-use scenarios. The DOE Office of Environmental Management approved these authorized limits on March 1, 2004. Historical soil monitoring conducted on and around the HRNM indicated soil concentrations of radionuclides were well below the authorized limits (Fritz et al. 2003). However, the historical sampling was done at a limited number of sampling locations. Therefore, additional soil sampling was conducted to determine if the concentrations of radionuclides in soil on the McGee Ranch-Riverlands and North Slope units were below the authorized limits. Sixty-seven soil samples were collected from the McGee Ranch-Riverlands and North Slope units. A software package (Visual Sample Plan) was used to plan the collection to assure an adequate number of samples were collected. The number of samples necessary to decide with a high level of confidence (99%) that the soil concentrations of radionuclides on the North Slope and McGee Ranch-Riverlands units did not exceed the authorized limits was determined to be 27. Additional soil samples were collected from areas suspected to have a potential for accumulation of radionuclides. This included samples collected from the riparian zone along the Columbia River, Savage Island, and other locations across the North Slope and McGee Ranch-Riverlands units. The 67 soil samples collected from the McGee Ranch-Riverlands and North Slope units all had concentrations of radionuclides far below the authorized limits established by the DOE. Statistical analysis of the results concluded that the Authorized Limits were not exceeded when total uncertainty was considered. The calculated upper confidence limit for each radionuclide measured in this study (which represents the value at which 99% of the measurements reside below with a 99% confidence level) was lower than the Authorized Limit for each radionuclide. The maximum observed soil concentrations for the radionuclides included in the authorized limits would result in a potential annual dose of 0.23 mrem assuming the most probable use scenario, a recreational visitor. This potential dose is well below the DOE 100-mrem/year dose limit for members of the public. Furthermore, the results of the biota dose assessment screen, which used the RESRAD biota code, indicated that the sum of fractions is less than one. This assumed soil concentrations equal to the maximum concentrations of radionuclides measured on the McGee Ranch-Riverlands and North Slope units’ in this study. Since the sum of fractions was less than 1, dose to terrestrial biota will not exceed the recommended biota dose limit for the soil concentrations measured in this study.« less

  4. Cleaning verification: A five parameter study of a Total Organic Carbon method development and validation for the cleaning assessment of residual detergents in manufacturing equipment.

    PubMed

    Li, Xue; Ahmad, Imad A Haidar; Tam, James; Wang, Yan; Dao, Gina; Blasko, Andrei

    2018-02-05

    A Total Organic Carbon (TOC) based analytical method to quantitate trace residues of clean-in-place (CIP) detergents CIP100 ® and CIP200 ® on the surfaces of pharmaceutical manufacturing equipment was developed and validated. Five factors affecting the development and validation of the method were identified: diluent composition, diluent volume, extraction method, location for TOC sample preparation, and oxidant flow rate. Key experimental parameters were optimized to minimize contamination and to improve the sensitivity, recovery, and reliability of the method. The optimized concentration of the phosphoric acid in the swabbing solution was 0.05M, and the optimal volume of the sample solution was 30mL. The swab extraction method was 1min sonication. The use of a clean room, as compared to an isolated lab environment, was not required for method validation. The method was demonstrated to be linear with a correlation coefficient (R) of 0.9999. The average recoveries from stainless steel surfaces at multiple spike levels were >90%. The repeatability and intermediate precision results were ≤5% across the 2.2-6.6ppm range (50-150% of the target maximum carry over, MACO, limit). The method was also shown to be sensitive with a detection limit (DL) of 38ppb and a quantitation limit (QL) of 114ppb. The method validation demonstrated that the developed method is suitable for its intended use. The methodology developed in this study is generally applicable to the cleaning verification of any organic detergents used for the cleaning of pharmaceutical manufacturing equipment made of electropolished stainless steel material. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Multiresidue analysis of sulfonamides in meat by supramolecular solvent microextraction, liquid chromatography and fluorescence detection and method validation according to the 2002/657/EC decision.

    PubMed

    Costi, Esther María; Sicilia, María Dolores; Rubio, Soledad

    2010-10-01

    A multiresidue method was described for determining eight sulfonamides, SAs (sulfadiazine, sulfamerazine, sulfamethoxypyridazine, sulfachloropyridazine, sulfadoxine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline) in animal muscle tissues (pork, chicken, turkey, lamb and beef) at concentrations below the maximum residue limit (100 μg kg(-1)) set by the European Commission. The method was based on the microextraction of SAs in 300-mg muscle samples with 1 mL of a supramolecular solvent made up of reverse micelles of decanoic acid (DeA) and posterior determination of SAs in the extract by LC/fluorescence detection, after in situ derivatization with fluorescamine. Recoveries were quantitative (98-109%) and matrix-independent, no concentration of the extracts was required, the microextraction took about 30 min and several samples could be simultaneously treated. Formation of multiple hydrogen bonds between the carboxylic groups of the solvent and the target SAs (hydrogen donor and acceptor sum between 9 and 11) were considered as the major forces driving microextraction. The method was validated according to the European Union regulation 2002/657/EC. Analytical performance in terms of linearity, selectivity, trueness, precision, stability of SAs, decision limit and detection capability were determined. Quantitation limits for the different SAs ranged between 12 μg kg(-1) and 44 μg kg(-1), they being nearly independent of matrix composition. Repeatability and reproducibility, expressed as relative standard deviation, were in the ranges 1.8-3.6% and 3.3-6.1%. The results of the validation process proved that the method is suitable for determining sulfonamide residues in surveillance programs. Copyright © 2010 Elsevier B.V. All rights reserved.

  6. Generation of High-Power High-Intensity Short X-Ray Free-Electron-Laser Pulses

    DOE PAGES

    Guetg, Marc W.; Lutman, Alberto A.; Ding, Yuantao; ...

    2018-01-03

    X-ray free-electron lasers combine a high pulse power, short pulse length, narrow bandwidth, and high degree of transverse coherence. Any increase in the photon pulse power, while shortening the pulse length, will further push the frontier on several key x-ray free-electron laser applications including single-molecule imaging and novel nonlinear x-ray methods. This Letter shows experimental results at the Linac Coherent Light Source raising its maximum power to more than 300% of the current limit while reducing the photon pulse length to 10 fs. As a result, this was achieved by minimizing residual transverse-longitudinal centroid beam offsets and beam yaw andmore » by correcting the dispersion when operating over 6 kA peak current with a longitudinally shaped beam.« less

  7. Generation of High-Power High-Intensity Short X-Ray Free-Electron-Laser Pulses

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Guetg, Marc W.; Lutman, Alberto A.; Ding, Yuantao

    X-ray free-electron lasers combine a high pulse power, short pulse length, narrow bandwidth, and high degree of transverse coherence. Any increase in the photon pulse power, while shortening the pulse length, will further push the frontier on several key x-ray free-electron laser applications including single-molecule imaging and novel nonlinear x-ray methods. This Letter shows experimental results at the Linac Coherent Light Source raising its maximum power to more than 300% of the current limit while reducing the photon pulse length to 10 fs. As a result, this was achieved by minimizing residual transverse-longitudinal centroid beam offsets and beam yaw andmore » by correcting the dispersion when operating over 6 kA peak current with a longitudinally shaped beam.« less

  8. Freestanding NiFe Oxyfluoride Holey Film with Ultrahigh Volumetric Capacitance for Flexible Asymmetric Supercapacitors.

    PubMed

    Liang, Kun; Marcus, Kyle; Yang, Zhenzhong; Zhou, Le; Pan, Hao; Bai, Yuanli; Du, Yingge; Engelhard, Mark H; Yang, Yang

    2018-01-01

    In this work, a freestanding NiFe oxyfluoride (NiFeOF) holey film is prepared by electrochemical deposition and anodic treatments. With the combination of good electrical conductivity and holey structure, the NiFeOF holey film offers superior electrochemical performance with maximum specific capacitance of 670 F cm -3 (134 mF cm -2 ), due to the following reasons: (i) The residual metal alloy framework can be used as the current collector to improve electrode conductivity. Moreover, the as-prepared freestanding NiFeOF holey film can be used as a supercapacitor electrode without reliance on binders and other additives. The residual metal alloy framework and binder-free electrode effectively reduce electrode resistance, thus improving electron transport. (ii) The highly interconnected holey structure and hierarchical pore distribution provide a high specific surface area to improve electron transport, enhancing rapid ion transport, and mitigating diffusion limitations throughout the holey film. (iii) The excellent mechanical characteristics facilitate flexibility and cyclability related performance. Additionally, the NiFeOF holey film presents exceptional electrochemical performance, showing that it is a promising alternative for small/microsize electronic devices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Two-dimensional coordination polymer matrix for solid-phase extraction of pesticide residues from plant Cordia salicifolia.

    PubMed

    de Carvalho, Pedro Henrique Viana; Barreto, Alysson Santos; Rodrigues, Marcelo O; Prata, Vanessa de Menezes; Alves, Péricles Barreto; de Mesquita, Maria Eliane; Alves, Severino; Navickiene, Sandro

    2009-06-01

    The 2D coordination polymer (infinity[Gd(DPA)(HDPA)]) was tested for extraction of acephate, chlorpropham, pirimicarb, bifenthrin, tetradifon, and phosalone from the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products, using GC/MS, SIM. Considering that there are no Brazilian regulations concerning maximum permissible pesticide residue concentrations in medicinal herbs, recovery experiments were carried out (seven replicates), at two arbitrary fortification levels (0.5 and 1.0 mg/kg), resulting in recoveries in range of 20 to 107.7% and SDRSDs were between 5.6 and 29.1% for infinity[Gd(DPA)(HDPA)] sorbent. Detection and quantification limits for herb ranged from 0.10 to 0.15 mg/kg and from 0.15 to 0.25 mg/kg, respectively, for the different pesticides studied. The developed method is linear over the range assayed, 0.5-10.0 microg/mL, with correlation coefficients ranging from 0.9975 to 0.9986 for all pesticides. Comparison between infinity[Gd(DPA)(HDPA)] sorbent and conventional sorbent (neutral alumina) showed similar performance of infinity[Gd(DPA)(HDPA)] polymeric sorbent for three (bifenthrin, tetradifon, and phosalone) out of six pesticides tested.

  10. Antibiotic, Pesticide, and Microbial Contaminants of Honey: Human Health Hazards

    PubMed Central

    Al-Waili, Noori; Salom, Khelod; Al-Ghamdi, Ahmed; Ansari, Mohammad Javed

    2012-01-01

    Agricultural contamination with pesticides and antibiotics is a challenging problem that needs to be fully addressed. Bee products, such as honey, are widely consumed as food and medicine and their contamination may carry serious health hazards. Honey and other bee products are polluted by pesticides, heavy metals, bacteria and radioactive materials. Pesticide residues cause genetic mutations and cellular degradation and presence of antibiotics might increase resistant human or animal's pathogens. Many cases of infant botulisms have been attributed to contaminated honey. Honey may be very toxic when produced from certain plants. Ingestion of honey without knowing its source and safety might be problematic. Honey should be labeled to explore its origin, composition, and clear statement that it is free from contaminants. Honey that is not subjected for analysis and sterilization should not be used in infants, and should not be applied to wounds or used for medicinal purposes. This article reviews the extent and health impact of honey contamination and stresses on the introduction of a strict monitoring system and validation of acceptable minimal concentrations of pollutants or identifying maximum residue limits for bee products, in particular, honey. PMID:23097637

  11. Determination of triazine herbicides and their metabolites in multiple medicinal parts of traditional Chinese medicines using streamlined pretreatment and UFLC-ESI-MS/MS.

    PubMed

    Liu, Congmin; Dou, Xiaowen; Zhang, Lei; Li, Qian; Qin, Jia'an; Duan, Yaping; Yang, Meihua

    2018-01-01

    A rapid, sensitive, and reliable ultra-fast liquid chromatography combined with electrospray ionization tandem mass spectrometry (UFLC-ESI-MS/MS) method was established and applied to simultaneous determination of 31 triazine herbicides and their metabolites in multiple medicinal parts of traditional Chinese medicines (TCMs). A streamlined pretreatment approach using one-step extraction and dilution was proposed, which provided high-throughput processing, excellent recovery, and negligible interference. Afterwards, multiple-reaction monitoring (MRM) and information-dependent acquisition (IDA) triggered enhanced product ion spectra (EPI) was adopted to identify and quantify the targets in a single analysis. The optimized method was then validated according to the guidelines of the European Commission for the following parameters: Matrix effects, specificity, accuracy, precision, linearity, range, and stability. The LOD and LOQ for the 31 triazine herbicides were 0.1-10 μg kg -1 and 0.5-25 μg kg -1 , respectively. Recoveries at three concentration levels were within 67.9-120.3% with an associated precision RSD <20%. Using the proposed approach, trazines herbicides were determined from 44 commercially available TCMs. The detection rate of triazine herbicides residues was 15.9% of the total samples. Among them, atrazine, simeton, and simetryn were found in the radix, herba, and seed TCMs with values far below the referenced maximum residue limits (MRLs), but no residues were detected in either the flos or fructus. Taken together, this method has the potential to provide a means for triazines screening in extensive matrices, thereby laying the foundation for pesticide registration on TCMs. Moreover, it has the potential to guide further triazine residue control in TCMs. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Risk of DDT residue in maize consumed by infants as complementary diet in southwest Ethiopia.

    PubMed

    Mekonen, Seblework; Lachat, Carl; Ambelu, Argaw; Steurbaut, Walter; Kolsteren, Patrick; Jacxsens, Liesbeth; Wondafrash, Mekitie; Houbraken, Michael; Spanoghe, Pieter

    2015-04-01

    Infants in Ethiopia are consuming food items such as maize as a complementary diet. However, this may expose infants to toxic contaminants like DDT. Maize samples were collected from the households visited during a consumption survey and from markets in Jimma zone, southwestern Ethiopia. The residues of total DDT and its metabolites were analyzed using the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method combined with dispersive solid phase extraction cleanup (d-SPE). Deterministic and probabilistic methods of analysis were applied to determine the consumer exposure of infants to total DDT. The results from the exposure assessment were compared with the health based guidance value in this case the provisional tolerable daily intake (PTDI). All maize samples (n=127) were contaminated by DDT, with a mean concentration of 1.770 mg/kg, which was far above the maximum residue limit (MRL). The mean and 97.5 percentile (P 97.5) estimated daily intake of total DDT for consumers were respectively 0.011 and 0.309 mg/kg bw/day for deterministic and 0.011 and 0.083 mg/kg bw/day for probabilistic exposure assessment. For total infant population (consumers and non-consumers), the 97.5 percentile estimated daily intake were 0.265 and 0.032 mg/kg bw/day from the deterministic and probabilistic exposure assessments, respectively. Health risk estimation revealed that, the mean and 97.5 percentile for consumers, and 97.5 percentile estimated daily intake of total DDT for total population were above the PTDI. Therefore, in Ethiopia, the use of maize as complementary food for infants may pose a health risk due to DDT residue. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Exposure to DDT and its metabolites from khat (Catha edulis) chewing: Consumers risk assessment from southwestern Ethiopia.

    PubMed

    Mekonen, Seblework; Ambelu, Argaw; Negassa, Belay; Spanoghe, Pieter

    2017-07-01

    Khat (Catha edulis) is one of the most consumed plant in the horn of African countries. However, it is a stimulant plant that has several side effects on the health of consumers. On top of that, the khat leaves used for human consumption are often contain contaminants such as pesticide residues. The present study aims to investigate the level of DDT residue and its metabolites (p'p-DDE, p'p-DDD, o'p-DDT and p'p-DDT) in khat samples and to undertake exposure assessment to consumers. The khat samples were collected from local markets in southwestern Ethiopia. Consumption survey was undertaken using 24 h recall method for both male and female khat consumers. The finding showed that 80% of the khat samples contained DDT and its metabolites. Some of the residues were above the maximum residue limit (MRL) set by Food and Agricultural Organization (FAO). The concentration of p'p-DDE and p'p-DDT in khat were in the range of 0.033-0.113 and 0.010-0.026 mg/kg, respectively. High concentration of the metabolite (p'p-DDE) compared to the parent compound (p'p-DDT) revealed the historical use of DDT in the study area. Probabilistic exposure analysis indicated that the mean and 97.5 percentile (P97.5), of the estimated daily intake of total DDT were 0.002 and 0.006 mg/kg bw/day, respectively. The study concluded that khat consumers are exposed to the stimulant effect of the plant as well as DDT and its metabolites in Jimma zone. Copyright © 2017 Elsevier Inc. All rights reserved.

  14. Determination of sulfadiazine, trimethoprim, and N(4) -acetyl-sulfadiazine in fish muscle plus skin by Liquid Chromatography-Mass Spectrometry. Withdrawal-time calculation after in-feed administration in gilthead sea bream (Sparus aurata L.) fed two different diets.

    PubMed

    Zonaras, V; Tyrpenou, A; Alexis, M; Koupparis, M

    2016-10-01

    This study presents a depletion study for sulfadiazine and trimethoprim in muscle plus skin of gilthead sea bream (Sparus aurata L.). N(4) -acetyl-sulfadiazine, the main metabolite of sulfadiazine (SDZ), was also examined. The fish were held in seawater at a temperature of 24-26 °C. SDZ and trimethoprim (TMP) were administered orally with medicated feed for five consecutive days at daily doses of 25 mg SDZ and 5 mg TMP per kg of fish body weight per day. Two different diets, fish oil- and plant oil-based diets, were investigated. Ten fish were sampled at each of the days 1, 3, 5, 6, 8, 9, 10, and 12 after the start of veterinary medicine administration. However for the calculation of the withdrawal periods, sampling day 1 was set as 24 h after the last dose of the treatment. Fish samples were analyzed for SDZ, TMP, and acetyl-sulfadiazine (AcSDZ) residues by liquid chromatography-mass spectrometry. SDZ and TMP concentrations declined rapidly from muscle plus skin. Considering a maximum residue limit of 100 μg/kg for the total of sulfonamides and 50 μg/kg for TMP residues in fish muscle plus skin, the withdrawal periods of the premix trimethoprim-sulfadiazine 50% were calculated as 5 and 6 days, at 24-26 °C, in fish oil (FO) and plant oil (PO) groups, respectively. The investigation of this work is important to protect consumers by controlling the undesirable residues in fish. © 2016 John Wiley & Sons Ltd.

  15. Analysis of 27 antibiotic residues in raw cow's milk and milk-based products--validation of Delvotest® T.

    PubMed

    Bion, Cindy; Beck Henzelin, Andrea; Qu, Yajuan; Pizzocri, Giuseppe; Bolzoni, Giuseppe; Buffoli, Elena

    2016-01-01

    Delvotest® T was evaluated for its capability at detecting residues of 27 antibiotics in raw cow's milk and in some dairy ingredients (skimmed and full-cream milk powders). The kit was used as a screening tool for the qualitative determination of antibiotics from different families in a single test. Results delivered by such a method are expressed as 'positive' or 'negative', referring to the claimed screening target concentration (STC). Validation was conducted according to the European Community Reference Laboratories' (CRLs) residues guidelines of 20 January 2010 and performed by two laboratories, one located in Europe and the other in Asia. Five criteria were evaluated including detection capability at STC, false-positive (FP) rate, false-negative (FN) rate, robustness and cross-reactivity using visual reading and Delvoscan®. STCs were set at or below the corresponding maximum residue limit (MRL), as fixed by European Regulation EC No. 37/2010. Four antibiotics (nafcillin, oxytetracycline, tetracycline and rifaximin) out of 27 had a false-negative rate ranging from 1.7% to 4.9%; however, it was still compliant with the CRLs' requirements. Globally, Delvotest T can be recommended for the analysis of the surveyed antibiotics in raw cow's milk, skimmed and full-cream milk powders. Additional compounds were tested such as sulfamethazine, spiramycin and erythromycin; however, detection at the corresponding MRL was not achievable and these compounds were removed from the validation. Other drugs from the sulfonamide, aminoglycoside or macrolide families not detected by the test at the MRL were not evaluated in this study. Regarding the reliability of this rapid test to milk-based preparations, additional experiments should be performed on a larger range of compounds and samples to validate the Delvotest T in such matrices.

  16. Differential effects of peroxynitrite on contractile protein properties in fast- and slow-twitch skeletal muscle fibers of rat.

    PubMed

    Dutka, T L; Mollica, J P; Lamb, G D

    2011-03-01

    Oxidative modification of contractile proteins is thought to be a key factor in muscle weakness observed in many pathophysiological conditions. In particular, peroxynitrite (ONOO(-)), a potent short-lived oxidant, is a likely candidate responsible for this contractile dysfunction. In this study ONOO(-) or 3-morpholinosydnonimine (Sin-1, a ONOO(-) donor) was applied to rat skinned muscle fibers to characterize the effects on contractile properties. Both ONOO(-) and Sin-1 exposure markedly reduced maximum force in slow-twitch fibers but had much less effect in fast-twitch fibers. The rate of isometric force development was also reduced without change in the number of active cross bridges. Sin-1 exposure caused a disproportionately large decrease in Ca(2+) sensitivity, evidently due to coproduction of superoxide, as it was prevented by Tempol, a superoxide dismutase mimetic. The decline in maximum force with Sin-1 and ONOO(-) treatments could be partially reversed by DTT, provided it was applied before the fiber was activated. Reversal by DTT indicates that the decrease in maximum force was due at least in part to oxidation of cysteine residues. Ascorbate caused similar reversal, further suggesting that the cysteine residues had undergone S-nitrosylation. The reduction in Ca(2+) sensitivity, however, was not reversed by either DTT or ascorbate. Western blot analysis showed cross-linking of myosin heavy chain (MHC) I, appearing as larger protein complexes after ONOO(-) exposure. The findings suggest that ONOO(-) initially decreases maximum force primarily by oxidation of cysteine residues on the myosin heads, and that the accompanying decrease in Ca(2+) sensitivity is likely due to other, less reversible actions of hydroxyl or related radicals.

  17. Prediction of active sites of enzymes by maximum relevance minimum redundancy (mRMR) feature selection.

    PubMed

    Gao, Yu-Fei; Li, Bi-Qing; Cai, Yu-Dong; Feng, Kai-Yan; Li, Zhan-Dong; Jiang, Yang

    2013-01-27

    Identification of catalytic residues plays a key role in understanding how enzymes work. Although numerous computational methods have been developed to predict catalytic residues and active sites, the prediction accuracy remains relatively low with high false positives. In this work, we developed a novel predictor based on the Random Forest algorithm (RF) aided by the maximum relevance minimum redundancy (mRMR) method and incremental feature selection (IFS). We incorporated features of physicochemical/biochemical properties, sequence conservation, residual disorder, secondary structure and solvent accessibility to predict active sites of enzymes and achieved an overall accuracy of 0.885687 and MCC of 0.689226 on an independent test dataset. Feature analysis showed that every category of the features except disorder contributed to the identification of active sites. It was also shown via the site-specific feature analysis that the features derived from the active site itself contributed most to the active site determination. Our prediction method may become a useful tool for identifying the active sites and the key features identified by the paper may provide valuable insights into the mechanism of catalysis.

  18. 21 CFR 184.1259 - Cocoa butter substitute.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... material incorporated by reference may be obtained from the AOAC INTERNATIONAL, 481 North Frederick Ave... in accordance with good manufacturing practice. (7) Residual methanol—5 parts per million maximum. (8...

  19. 21 CFR 184.1259 - Cocoa butter substitute.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... material incorporated by reference may be obtained from the AOAC INTERNATIONAL, 481 North Frederick Ave... in accordance with good manufacturing practice. (7) Residual methanol—5 parts per million maximum. (8...

  20. 20 CFR 228.14 - Family maximum.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 20 Employees' Benefits 1 2011-04-01 2011-04-01 false Family maximum. 228.14 Section 228.14... SURVIVOR ANNUITIES The Tier I Annuity Component § 228.14 Family maximum. (a) Family maximum defined. Under... person's earnings record is limited. This limited amount is called the family maximum. The family maximum...

  1. 20 CFR 228.14 - Family maximum.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 20 Employees' Benefits 1 2010-04-01 2010-04-01 false Family maximum. 228.14 Section 228.14... SURVIVOR ANNUITIES The Tier I Annuity Component § 228.14 Family maximum. (a) Family maximum defined. Under... person's earnings record is limited. This limited amount is called the family maximum. The family maximum...

  2. Persistence and risk assessment of emamectin benzoate residues on okra fruits and soil.

    PubMed

    Jyot, Gagan; Mandal, Kousik; Chahil, G S; Singh, Balwinder

    2014-08-01

    Emamectin benzoate, a synthetic derivative of abamectin, is found effective against fruit borer and jassid in okra crops. The present studies were carried out to study the dissipation pattern of emamectin benzoate on okra and to suggest a suitable waiting period for the safety of consumers. Following three applications of emamectin benzoate (Proclaim 5 SG) at 68.1 and 136.2 g a.i. ha-1, the average initial deposits of emamectin benzoate were observed to be 0.22 and 0.42mg kg-1, respectively. These residues dissipated below the limit of quantification (LOQ) of 0.05 mg kg-1 after 5 days at both the dosages. Soil samples collected after 15 days did not reveal the presence of emamectin benzoate at LOQ of 0.05 mg kg-1. Acceptable daily intake (ADI) of emamectin benzoate is 0.0005 mg kg-1 body weight day-1, which means an adult of 55 kg weight can safely tolerate an intake of 27.50 microg emamectin benzoate. Assuming an average consumption of 80 g okra fruit and multiplying it by average and maximum residues observed on 0 day at recommended dosage, the intake of emamectin benzoate comes out to be about 20 Itg and these values are quite safe in comparison to its ADI. These studies, therefore, suggest that the use of emamectin benzoate at the minimum effective dosages do not seem to pose any hazards to the consumers if a waiting period of 1 day is observed.

  3. The role of validated analytical methods in JECFA drug assessments and evaluation for recommending MRLs.

    PubMed

    Boison, Joe O

    2016-05-01

    The Joint Food and Agriculture Organization and World Health Organization (FAO/WHO) Expert Committee on Food Additives (JECFA) is one of three Codex committees tasked with applying risk analysis and relying on independent scientific advice provided by expert bodies organized by FAO/WHO when developing standards. While not officially part of the Codex Alimentarius Commission structure, JECFA provides independent scientific advice to the Commission and its specialist committees such as the Codex Committee on Residues of Veterinary Drugs in Foods (CCRVDF) in setting maximum residue limits (MRLs) for veterinary drugs. Codex methods of analysis (Types I, II, III, and IV) are defined in the Codex Procedural Manual as are criteria to be used for selecting methods of analysis. However, if a method is to be used under a single laboratory condition to support regulatory work, it must be validated according to an internationally recognized protocol and the use of the method must be embedded in a quality assurance system in compliance with ISO/IEC 17025:2005. This paper examines the attributes of the methods used to generate residue depletion data for drug registration and/or licensing and for supporting regulatory enforcement initiatives that experts consider to be useful and appropriate in their assessment of methods of analysis. Copyright © 2016 Her Majesty the Queen in Right of Canada. Drug Testing and Analysis © 2016 John Wiley & Sons, Ltd. © 2016 Her Majesty the Queen in Right of Canada. Drug Testing and Analysis © 2016 John Wiley & Sons, Ltd.

  4. Residue behavior and risk assessment of imidacloprid applied on greenhouse-cultivated strawberries under different application conditions.

    PubMed

    Cang, Tao; Sun, Caixia; Zhao, Hua; Tang, Tao; Zhang, Changpeng; Yu, Ruixian; Wang, Xinquan; Wang, Qiang; Dai, Fen; Zhao, Xueping

    2018-02-01

    A risk assessment for imidacloprid applied on strawberries under different conditions was performed after residue determination using the quick, cheap, effective, rugged, and safe (QuEChERS) method. The application conditions were varied according to the applied dosage, addition of a plant oil or organosilicon surfactant, water volume, and sprayer type. The degradation dynamics of imidacloprid on strawberries followed first-order kinetics. At applied doses of 30-60 g a.i. ha -1 , the half-lives of imidacloprid were 2.89-3.46, 1.98-3.65, and 2.57-2.77 days after application without a surfactant or with a plant oil or organosilicon surfactant, respectively. For water volumes of 112.5, 225, 450, 675, and 900 L ha -1 , the half-lives of imidacloprid applied in the presence of the plant oil surfactant were 3.30, 7.70, 5.33, 7.70, and 6.30 days, respectively. The half-lives after application with a knapsack mist duster, electric sprayer, and manual sprayer were 2.16, 5.77, and 7.70 days, respectively. The health risk assessment revealed risk quotients less than 1 in all cases, indicating that the application of imidacloprid poses a low health risk to humans after a pre-harvest interval of 10 days under our application conditions. The risk assessment results can provide reference data for setting a reasonable maximum residue limit for imidacloprid on strawberries in China.

  5. Protein and Peptide Gas-phase Structure Investigation Using Collision Cross Section Measurements and Hydrogen Deuterium Exchange

    NASA Astrophysics Data System (ADS)

    Khakinejad, Mahdiar

    Protein and peptide gas-phase structure analysis provides the opportunity to study these species outside of their explicit environment where the interaction network with surrounding molecules makes the analysis difficult [1]. Although gas-phase structure analysis offers a unique opportunity to study the intrinsic behavior of these biomolecules [2-4], proteins and peptides exhibit very low vapor pressures [2]. Peptide and protein ions can be rendered in the gas-phase using electrospray ionization (ESI) [5]. There is a growing body of literature that shows proteins and peptides can maintain solution structures during the process of ESI and these structures can persist for a few hundred milliseconds [6-9]. Techniques for monitoring gas-phase protein and peptide ion structures are categorized as physical probes and chemical probes. Collision cross section (CCS) measurement, being a physical probe, is a powerful method to investigate gas-phase structure size [3, 7, 10-15]; however, CCS values alone do not establish a one to one relation with structure(i.e., the CCS value is an orientationally averaged value [15-18]. Here we propose the utility of gas-phase hydrogen deuterium exchange (HDX) as a second criterion of structure elucidation. The proposed approach incudes extensive MD simulations to sample biomolecular ion conformation space with the production of numerous, random in-silico structures. Subsequently a CCS can be calculated for these structures and theoretical CCS values are compared with experimental values to produce a pool of candidate structures. Utilizing a chemical reaction model based on the gas-phase HDX mechanism, the HDX kinetics behavior of these candidate structures are predicted and compared to experimental results to nominate the best in-silico structures which match (chemically and physically) with experimental observations. For the predictive approach to succeed, an extensive technique and method development is essential. To combine CCS measurements and gas-phase HDX studies at the amino acid residue level, for the first time a drift tube is connected to a linear ion trap (LIT) with electron transfer dissociation (ETD) capability[19, 20]. In this manner CCS and per-residue deuterium uptake measurements for a model peptide carried out successfully[19]. In this study, the gas-phase conformations of electrosprayed ions of the model peptide KKDDDDIIKIIK have been examined. Using ion structures obtained from molecular dynamics (MD) simulation and considering charge-site/exchange-site density the level of the maximum total deuterium uptake for the gas-phase ions is explained. Also a new hydrogen accessibility scoring (HAS) model that includes two distance calculations (charge site to carbonyl group and carbonyl group to exchange site) is applied to the in-silico structures to describe the expected HDX behavior for these structures. Further investigation to improve the accuracy of the model is accomplished by a "per-residue" HDX kinetics study of the model peptide [21]. In this study, the ion residence time and the deuterium uptake of each residue is measured at different partial pressures of D2O. Subsequently the contribution each residue to the overall HDX rate of the intact peptide ion is calculated. These rate contributions of the residues exhibit a better fit to HAS than their maximum deuterium uptake. Proteins and peptides with very frequent acidic residue in their sequence provide very poor signal levels when employing positive polarity ESI. Also, the comparison of protonated and deprotonated ions of these biomolecules offers the potential to provide a better structural characterization [22]. Per-residue deuterium uptake values resulting from collision-induced dissociation (CID) of the model peptide KKDDDDIIKIIK were used to investigated the degree of hydrogen deuterium scrambling for deprotonated ions [23]. Remarkably, limited isotopic scrambling was observed in this study of this small model peptide. This data and the per-residue deuterium uptake of the triply-protonated model peptide Acetyl-PAAAAKAAAAKAAAAKAAAAK are exploited to propose a lemma to allocate protonation and deprotonation sites for peptide ions in the gas-phase. Insulin ions, as a small protein model system, are examined to investigate the relation of the maximum deuterium uptake value for each insulin chain to the exposed surface area of each insulin subunit [22]. The results show that the methodology can be applied on the protein complexes to provide information about the exposed surface area of each subunit.

  6. Survey of Veterinary Drug Residues in Raw Milk in Hebei Province, China.

    PubMed

    Han, Rong-Wei; Yu, Zhong-Na; Zhen, Tian-Yuan; Wang, Jun

    2017-10-17

    The objective of this study was to investigate the occurrence of veterinary drug residues in raw milk from Hebei, the second-largest dairy production province in the People's Republic of China. A total of 192 raw milk samples were collected from 64 milk stations in seven districts. Twenty-eight veterinary drug residues were analyzed by ultraperformance liquid chromatography with tandem mass spectrometry based on a China National Standard. Raw milk samples with multiple residues of veterinary drugs were not found in the present study. Residues of four veterinary drugs, penicillin G, sulfacetamide, trimethoprim, and lincomycin, were detected in 12 (6.25%) raw milk samples, with detection ratios of 1.04, 0.52, 3.13, and 1.56%, respectively. All veterinary drug residues detected were under the maximum residue levels as regulated by China, the European Union, the United States, and the Codex Alimentarius Commission. In general, raw milk from Hebei province was considered relatively safe for human consumption because of the low prevalence of veterinary drug residues. However, stringent control measurements for veterinary drug residues in raw milk are required because some veterinary drugs were detected in milk from some areas of Hebei province.

  7. 40 CFR 180.184 - Linuron; tolerances for residues.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... Linuron; tolerances for residues. (a) General. Tolerances are established for residues of the herbicide.... Time-limited tolerances are established for residues of the herbicide linuron [3-(3,4-dichlorophenyl)-1... herbicide linuron (3-(3,4-dichlorophenyl)-1-methoxy-1-methylurea), including its metabolites and degradates...

  8. Focus on agricultural residues: Microstructure of almond hull (abstract)

    USDA-ARS?s Scientific Manuscript database

    Agricultural residues have historically been used as animal feed or burned for disposal. These residues, therefore, have little economic value and may end up becoming disposal problems because tighter air quality control measures may limit burning of the residues. Therefore, value-added products mad...

  9. A 3-year survey of Italian honey bee-collected pollen reveals widespread contamination by agricultural pesticides.

    PubMed

    Tosi, Simone; Costa, Cecilia; Vesco, Umberto; Quaglia, Giancarlo; Guido, Giovanni

    2018-02-15

    Honey bee (Apis mellifera L.) health is compromised by complex interactions between multiple stressors, among which pesticides play a major role. To better understand the extent of honey bee colonies' exposure to pesticides in time and space, we conducted a survey by collecting corbicular pollen from returning honey bee foragers in 53 Italian apiaries during the active beekeeping season of 3 subsequent years (2012-2014). Of 554 pollen samples analysed for pesticide residues, 62% contained at least one pesticide. The overall rate of multiresidual samples (38%) was higher than the rate of single pesticide samples (24%), reaching a maximum of 7 pesticides per sample (1%). Over 3years, 18 different pesticides were detected (10 fungicides and 8 insecticides) out of 66 analysed. Pesticide concentrations reached the level of concern for bee health (Hazard Quotient (HQ) higher than 1000) at least once in 13% of the apiaries and exceeded the thresholds of safety for human dietary intake (Acute Reference Dose (ARfD), the Acceptable Daily Intake (ADI), and the Maximum Residue Limit (MRL)) in 39% of the analysis. The pesticide which was most frequently detected was the insecticide chlorpyrifos (30% of the samples overall, exceeding ARfD, ADI, or MRL in 99% of the positive ones), followed by the fungicides mandipropamid (19%), metalaxyl (16%), spiroxamine (15%), and the neonicotinoid insecticide imidacloprid (12%). Imidacloprid had also the highest HQ level (5054, with 12% of its positive samples with HQ higher than 1000). This 3year survey provides further insights on the contamination caused by agricultural pesticide use on honey bee colonies. Bee-collected pollen is shown to be a valuable tool for environmental monitoring, and for the detection of illegal uses of pesticides. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Pesticides data-collection activities of the U.S. Geological Survey in Texas

    USGS Publications Warehouse

    Manigold, Douglas B.

    1974-01-01

    In 1965, the U.S. Geological Survey initiated a monthly monitoring program on 3 streams in Texas, screening for 9 of the more commonly used organochlorine insecticides: Aldrin, DDD, DDE , DDT, dieldrin, endrin, heptachlor, heptachlor epoxide, and lindane. Later, the herbicides 2,4-D; 2,4,5-T; and silvex were added. In 1967 a quarterly monitoring program was initiated at 26 sites on the principal streams of the State and a survey of the occurrence of pesticide residues in ground water. By 1970, the Geological Survey had developed methods for measuring pesticide residues in sediment, and in that year, the quarterly analysis of stream-bottom materials at 39 sites was added to the data collection program. Geological Survey pesticide data for 108 sites on nontidal reaches of streams in Texas have been summarized by Rawson (1974). The pesticides studied are widely distributed in surface waters in Texas. The most widely distributed chlorinated-hydrocarbon insecticides were dieldrin at 77 sites, DDT at 67 sites, lindane at 59 sites, and chlordane at 38 sites. The most widely distributed phosphorothioate insecticide was diazinon, which was detected at 80 sites. Small amounts of each of the chlorinated-hydrocarbon herbicides were widely distributed (2,4,5-T at 96 sites, 2,4-D at 78 sites, and Silvex at 47 sites). Although only chlordane, in 2 samples from 1 site exceeded the maximum limit recommended for water to be used for public supply, 1 or more pesticides in at least 1 sample from 57 sites exceeded the maximum environmental level for marine waters recommended by the National Technical Advisory Committee. (Woodard-USGS)

  11. Safe apples for baby-food production: survey of pesticide treatment regimes leaving minimum residues.

    PubMed

    Ticha, Jana; Hajslova, Jana; Kovalczuk, Tomas; Jech, Martin; Honzicek, Jiri; Kocourek, Vladimir; Lansky, Miroslav; Kloutvorova, Jana; Falta, Vladan

    2007-06-01

    A total of 19 pesticide preparations were used according to agricultural practice in six trials in apple orchards. Using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), premature Golden Delicious apples collected 64, 50, 36 days before harvest and mature fruit were examined for residues of active ingredients. No residues of triflumuron, triazamate, chlorpyrifos, etofenprox, fenoxycarb, kresoxim-methyl, cyprodinyl, difenoconazole or thiram were detected in the first sampling. Also, the levels of chlorpyrifos-methyl, penconazole, tebuconazole and tolylfluanid dropped during the pre-harvest interval. Detectable residues of pyridaben, thiacloprid, trifloxystrobin and tetraconazole in harvested fruits were below 0.01 mg kg(-1), which is the maximum concentration of residues acceptable by baby-food producers in any raw material. The only residues exceeding this concentration were captan and teflubenzuron. Based on the data, farmers can choose pesticides for optimal treatment of plants, while enabling growth of a safe crop suitable for baby-food production.

  12. 4D-PET reconstruction using a spline-residue model with spatial and temporal roughness penalties

    NASA Astrophysics Data System (ADS)

    Ralli, George P.; Chappell, Michael A.; McGowan, Daniel R.; Sharma, Ricky A.; Higgins, Geoff S.; Fenwick, John D.

    2018-05-01

    4D reconstruction of dynamic positron emission tomography (dPET) data can improve the signal-to-noise ratio in reconstructed image sequences by fitting smooth temporal functions to the voxel time-activity-curves (TACs) during the reconstruction, though the optimal choice of function remains an open question. We propose a spline-residue model, which describes TACs as weighted sums of convolutions of the arterial input function with cubic B-spline basis functions. Convolution with the input function constrains the spline-residue model at early time-points, potentially enhancing noise suppression in early time-frames, while still allowing a wide range of TAC descriptions over the entire imaged time-course, thus limiting bias. Spline-residue based 4D-reconstruction is compared to that of a conventional (non-4D) maximum a posteriori (MAP) algorithm, and to 4D-reconstructions based on adaptive-knot cubic B-splines, the spectral model and an irreversible two-tissue compartment (‘2C3K’) model. 4D reconstructions were carried out using a nested-MAP algorithm including spatial and temporal roughness penalties. The algorithms were tested using Monte-Carlo simulated scanner data, generated for a digital thoracic phantom with uptake kinetics based on a dynamic [18F]-Fluromisonidazole scan of a non-small cell lung cancer patient. For every algorithm, parametric maps were calculated by fitting each voxel TAC within a sub-region of the reconstructed images with the 2C3K model. Compared to conventional MAP reconstruction, spline-residue-based 4D reconstruction achieved  >50% improvements for five of the eight combinations of the four kinetics parameters for which parametric maps were created with the bias and noise measures used to analyse them, and produced better results for 5/8 combinations than any of the other reconstruction algorithms studied, while spectral model-based 4D reconstruction produced the best results for 2/8. 2C3K model-based 4D reconstruction generated the most biased parametric maps. Inclusion of a temporal roughness penalty function improved the performance of 4D reconstruction based on the cubic B-spline, spectral and spline-residue models.

  13. Seismic performance of the typical RC beam-column joint subjected to repeated earthquakes

    NASA Astrophysics Data System (ADS)

    Hassanshahi, Omid; Majid, Taksiah A.; Lau, Tze Liang; Yousefi, Ali; Tahara, R. M. K.

    2017-10-01

    It is common that a building experience repeated earthquakes throughout its lifetime. Such earthquake is capable of creating severe damage in primary elements of the building due to accumulation of inelastic displacement from repetition. The present study focuses on the influence of repeated earthquakes on a typical Reinforced Concrete (RC) beam-column joint, especially on the maximum inelastic displacement demand and maximum residual displacement. For this purpose, the capability of nonlinear modelling in simulating the hysteretic behaviour of the prototype experimental specimen is first determined using RUAUMOKO. A nonlinear Incremental Dynamic Analysis (IDA) on the verified model is then carried out in order to estimate with maximum accuracy the ultimate load bearing capacity to progressive collapse of the RC joint under investigation. Twenty ground motions are selected, and single (C1), double (C2), and triple (C3) event of synthetic repeated earthquakes are then considered. The results show that the repeated earthquakes significantly increase the inelastic demand of the RC joint. On average, relative increment of maximum inelastic displacement demand is experienced about 28.9% and 39.4% when C2 and C3 events of repeated earthquakes are induced, respectively. Residual displacements for repeated earthquakes are also significantly higher than that for single earthquakes.

  14. [Finite element analysis of the stress distribution of two-piece post crown with different adhesives ].

    PubMed

    He, Lihui; Liu, Lijie; Gao, Bei; Gao, Shang; Chen, Yifu; Zhihui, Liu

    2013-08-01

    To establish three-dimensional finite element model of two-piece post crown to the mandibular first molar residual roots, and analyze the stress distribution characteristic to the residual roots with different adhesives, so as to get the best combination under different conditions. The complete mandibular first molar in vitro was selected, the crown was removed along the cemento-enamel junction, then the residual roots were scanned by CT. CT images were imported into a reverse engineering software, and the three-dimensional finite element model of the mandibular first molar residual roots was reconstructed. Titanium two-piece post crown of the mandibular first molar residual roots was produced, then was scanned by CT. The model was reconstructed and assembled by MIMICS. The stress distribution of the root canal and root section under the vertical load and lateral load with different bonding systems were analyzed. Three-dimensional finite element model of two-piece post crown to the mandibular first molar residual roots was established. With the increasing of elastic modulus of the adhesives, the maximum stress within the root canal was also increasing. Elastic modulus of zinc phosphate was the biggest, so the stress within the root canal was the biggest; elastic modulus of Superbond C&B was the smallest, so the stress within the root canal was the smallest. Lateral loading stress was much larger than the vertical load. Under vertical load, the load on the root section was even with different bonding systems. Under lateral load, the maximum stress was much larger than the vertical load. The stress on the root section was minimum using zinc phosphate binder, and the stress on the root section was maximum using Superbond C&B. In two-piece post crown restorations, there is significant difference between different adhesives on tooth protection. When the tooth structure of the root canal orifices is weak, in order to avoid the occurrence of splitting, the larger elastic modulus bonding system is the first choice, such as zinc phosphate binder. When the resistance form of the root canal orifices is good enough but the root is too weak, it is suggested that the smaller elastic modulus bonding system is the first choice, such as Superbond C&B.

  15. 40 CFR 432.42 - Effluent limitations attainable by the application of the best practicable control technology...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... at any time. 4 No maximum monthly average limitation. 5 May be measured as hexane extractable... limitations: (1) All facilities must achieve the following effluent limitations for ammonia (as N): Effluent Limitations [BPT] Regulated parameter Maximum daily 1 Maximum monthly avg. 1 Ammonia (as N) 8.0 4.0 1 mg/L...

  16. 40 CFR 432.42 - Effluent limitations attainable by the application of the best practicable control technology...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... at any time. 4 No maximum monthly average limitation. 5 May be measured as hexane extractable... limitations: (1) All facilities must achieve the following effluent limitations for ammonia (as N): Effluent Limitations [BPT] Regulated parameter Maximum daily 1 Maximum monthly avg. 1 Ammonia (as N) 8.0 4.0 1 mg/L...

  17. 40 CFR 432.42 - Effluent limitations attainable by the application of the best practicable control technology...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... at any time. 4 No maximum monthly average limitation. 5 May be measured as hexane extractable... limitations: (1) All facilities must achieve the following effluent limitations for ammonia (as N): Effluent Limitations [BPT] Regulated parameter Maximum daily 1 Maximum monthly avg. 1 Ammonia (as N) 8.0 4.0 1 mg/L...

  18. 40 CFR 432.42 - Effluent limitations attainable by the application of the best practicable control technology...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... at any time. 4 No maximum monthly average limitation. 5 May be measured as hexane extractable... limitations: (1) All facilities must achieve the following effluent limitations for ammonia (as N): Effluent Limitations [BPT] Regulated parameter Maximum daily 1 Maximum monthly avg. 1 Ammonia (as N) 8.0 4.0 1 mg/L...

  19. 40 CFR 432.42 - Effluent limitations attainable by the application of the best practicable control technology...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... at any time. 4 No maximum monthly average limitation. 5 May be measured as hexane extractable... limitations: (1) All facilities must achieve the following effluent limitations for ammonia (as N): Effluent Limitations [BPT] Regulated parameter Maximum daily 1 Maximum monthly avg. 1 Ammonia (as N) 8.0 4.0 1 mg/L...

  20. Through-Thickness Residual Stress Profiles in Austenitic Stainless Steel Welds: A Combined Experimental and Prediction Study

    NASA Astrophysics Data System (ADS)

    Mathew, J.; Moat, R. J.; Paddea, S.; Francis, J. A.; Fitzpatrick, M. E.; Bouchard, P. J.

    2017-12-01

    Economic and safe management of nuclear plant components relies on accurate prediction of welding-induced residual stresses. In this study, the distribution of residual stress through the thickness of austenitic stainless steel welds has been measured using neutron diffraction and the contour method. The measured data are used to validate residual stress profiles predicted by an artificial neural network approach (ANN) as a function of welding heat input and geometry. Maximum tensile stresses with magnitude close to the yield strength of the material were observed near the weld cap in both axial and hoop direction of the welds. Significant scatter of more than 200 MPa was found within the residual stress measurements at the weld center line and are associated with the geometry and welding conditions of individual weld passes. The ANN prediction is developed in an attempt to effectively quantify this phenomenon of `innate scatter' and to learn the non-linear patterns in the weld residual stress profiles. Furthermore, the efficacy of the ANN method for defining through-thickness residual stress profiles in welds for application in structural integrity assessments is evaluated.

Top