Problem Definition Study on the Health Effects of Diethyleneglycol Dinitrate, Triethylenegycol Dinitrate, and Trimethylolethane Trinitrate and Their Respective Combustion Products

DTIC Science & Technology

1983-04-01

pento- barbital, it was only 321 (170-605, 95% confidence limits) mg/kg. Significant increases in pentobarbital sleep times were observed in rats...alka- line phosphatase, creatinine kinase, lactic dehydrogenase, and aspartate aminotransferase , and measurements of lactic dehydrogenase isoenzyme...pento- barbital sleep time, zoxazolamine paralysis time, and Metrazol toxicity were determined after treatment with the compound; the effect of the

Tissue sources of serum alkaline phosphatase in 34 hyperthyroid cats: a qualitative and quantitative study.

PubMed

Foster, D J; Thoday, K L

2000-02-01

The concentration of serum alkaline phosphatase (SALP) is commonly elevated in hyperthyroid cats. Agarose gel electrophoresis, in tris -barbital-sodium barbital buffer, with and without the separation enhancer neuraminidase, was used to investigate the sources of the constituent isoenzymes of SALP in serum samples from 34 hyperthyroid cats, comparing them to sera from five healthy cats and to tissue homogenates from liver, kidney, bone and duodenum. Contrary to previous reports, treatment of serum with neuraminidase made differentiation of the various isoenzymes more difficult to achieve. A single band corresponding to the liver isoenzyme (LALP) was found in 100 per cent of healthy cats. Eighty-eight per cent of the hyperthyroid cats showed two bands, corresponding to the liver and bone (BALP) isoenzymes while 12 per cent showed a LALP band alone. In hyperthyroid cats, there was a significant correlation between the serum L-thyroxine concentrations and the SALP concentrations. These findings suggest pathological changes in both bone and liver in most cases of feline thyrotoxicosis. Copyright 2000 Harcourt Publishers LtdCopyright 2000 Harcourt Publishers Ltd.

[On the history of barbiturates].

PubMed

Norn, Svend; Permin, Henrik; Kruse, Edith; Kruse, Poul R

2015-01-01

Throughout the history of humanity, numerous therapeutic agents have been employed for their sedative and hypnotic properties such as opium, henbane (Hyoscyamus niger) and deadly nightshade (Atropa belladonna), but also alcohol and wine. In the 19th century potassium bromide was introduced as a sedative - and antiepileptic drug and chloral hydrate as sedative-hypnotics. A new era was reached by the introduction of barbiturates. The story started with the chemist Adolf von Baeyer. His breakthrough in the synthesis of new agents as barbituric acid and indigo and his education of young chemists was of great importance for the science of organic chemistry and the development of the dye and medicine industry in the late 19th century. The next important step was the development of barbiturates. The pioneers were Josef von Mering and Emil Fischer. Using the Grimaux-method they synthesized various barbiturates. It was von Mering who got the idea of introducing ethyl groups in the inactive barbituric acid to obtain sedatives, but the synthesis was succeeded by the chemist Emil Fischer. Experiments with dogs clearly showed sedative and hypnotic effect of the barbiturates and the oral administration of barbital (Veronal) confirmed the effect in humans. Barbital was commercialized in 1903 and in 1911 phenobarbital (Luminal) was introduced in the clinic, and this drug showed hypnotic and antiepileptic effects. Thereafter a lot of new barbiturates appeared. Dangerous properties of the drugs were recognized as abuse, addiction, and poisoning. An optimum treatment of acute barbiturate intoxication was obtained by the "Scandinavian method", which was developed in the Poison Centre of the Bispebjerg Hospital in Copenhagen. The centre was established by Carl Clemmesen in 1949 and the intensive care treatment reduced the mortality of the admitted persons from 20% to less than 2%. To-day only a few barbiturates are used in connection with anaesthesia and for the treatment of epilepsy

Assessment of sensitization potential of monoterpenes using the rat popliteal lymph node assay.

PubMed

Friedrich, Karen; Delgado, Isabella F; Santos, Laísa M F; Paumgartten, Francisco J R

2007-08-01

The popliteal lymph node assay (PLNA) has been proposed as a screening test for detecting chemicals with potential of inducing allergic and auto-immune-like reactions in humans. In the present study, we used the rat PLNA to evaluate the immuno-sensitizing potential of 10 monoterpenes found in the essential oils of a variety of aromatic, edible and medicinal plants. The primary or direct PLNA was performed with the monoterpenes, and chlorpromazine (CPZ) and barbital were used as positive and negative controls, respectively. Female, 7-8 week-old Wistar rats were injected subcutaneously (50 microL) with the test substance (0.5, 2.5 or 5mg) into the right hind footpad while the contralateral footpad was injected with the vehicle (DMSO) alone. Weight (WI) and cellularity (CI) indices for draining PLNs were determined 7 days after treatment. PLNA was positive (WI >or= 2 and CI >or= 5) for CPZ, citral, alpha-terpinene, beta-myrcene and (-)-alpha-pinene, and negative for barbital, DMSO, (-)-menthol, 1,8-cineole, (+/-) citronellal, (+)-limonene, (+/-) camphor and terpineol. A secondary PLNA, a T-cell priming test, was carried out with the four substances that had been positive in the primary assay. Six weeks after being locally primed with 5 mg/paw, rats were sc injected into the same footpad with a dose (0.5 mg/paw) of the substance that had been previously found to be insufficient to cause a positive response. WI and CI were then calculated 4 and 7 days after the second injection. CPZ was also positive in the secondary assay thereby confirming that it is a sensitizing agent. Citral, alpha-terpinene, beta-myrcene and (-)-alpha-pinene, however, were negative in the secondary assay. In summary, citral, alpha-terpinene, beta-myrcene and (-)-alpha-pinene induced a clear immuno-stimulatory response due to their irritant properties but no monoterpene proved to be a sensitizing agent in the PLNA.

Determination of psilocybin in Psilocybe semilanceata by capillary zone electrophoresis.

PubMed

Pedersen-Bjergaard, S; Sannes, E; Rasmussen, K E; Tønnesen, F

1997-07-04

A capillary zone electrophoretic (CZE) method was developed for the rapid determination of psilocybin in Psilocybe semilanceata. Following a simple two step extraction with 3.0+2.0 ml methanol, the hallucinogenic compound was effectively separated from matrix components by CZE utilizing a 10 mM borate-phosphate running buffer adjusted to pH 11.5. The identity of psilocybin was confirmed by migration time information and by UV spectra, while quantitation was accomplished utilizing barbital as internal standard. The calibration curve for psilocybin was linear within 0.01-1 mg/ml, while intra-day and inter-day variations of quantitative data were 0.5 and 2.5% R.S.D., respectively. In addition to psilocybin, the method was also suitable for the determination of the structurally related compound baeocystin.

Study of the adsorbed layer on a solid electrode surface by specular reflection measurement

NASA Astrophysics Data System (ADS)

Kusu, Fumiyo; Takamura, Kiyoko

1985-07-01

Specular reflection measurements were carried out to study the adsorbed layers of certain heterocyclic compounds such as adenine, barbital, 2'-deoxyadenosine, phenobarbital, pyridine and thymine. When pyridine was present in 0.1M NaClO 4, a marked decrease in the reflectivity of a gold electrode was observed. In the potential range near the point of zero charge on the reflectivity-potential curve, the decrease was due to the adsorption of pyridine. Assuming the reflectivity change to be proportional to the surface coverage, the potential and concentration dependence of pyridine adsorption was determined and analysed on the basis of a Langmuir-type adsorption isotherm. The refractive indices and extinction coefficients for the adsorbed layers of the compounds investigated were evaluated using the observed reflectivity change, according to relations proposed by McIntyre and Aspnes.

Activity of respiratory system during laser irradiation of brain structures

NASA Astrophysics Data System (ADS)

Merkulova, N. A.; Sergeyeva, L. I.

1984-06-01

The performance of one of the principal links of the respiratory system, the respiratory center, was studied as a function of the exposure of the medulla oblongata and the sensomotor zone of the cerebral hemisphere cortex to low level laser irradiation in the red wavelength of the spectrum. Experiments were done on white rats under barbital anesthesia. Under such conditions a substantial effect was observed on the activity of the respiratory center. Laser light may display activating or inhibitory influences, in some cases the bilateral symmetry of the activity of the respiratory center is affected indicating deep changes in the integrative mechanism of the functioning of the right and left sides of the hemispheres. The laser beam effect depends on many factors: specific light properties, duration of the exposure, repetition of exposures, initial functional state of the CNS, etc.

Behavior and physiology of two different sow breeds in a farrowing environment during late 35-day lactation.

PubMed

Liu, Honggui; Yi, Ran; Wang, Chao; Zhao, Peng; Zhang, Mingyue; Xu, Shiwen; Bao, Jun

2018-01-01

To improve the overall welfare levels of sows and to reduce stress levels at late 35-day lactation, we selected targeted behavioral indicators that might be associated with stress. Therefore, we monitored and evaluated the adaptive capability of two different breeds of sows to the farrowing environment. In this study, Damin sows (Large White × Min pig sows, n = 20) and Large White sows (n = 20) were farrowed in individual pens. Saliva was collected and tested for cortisol density at -15 min, and then at +15, 30, 60, 90, 120, 180 and 240 min after an adrenocorticotropic hormone (ACTH) stimulation test conducted at 20, 27 and 34 d post-partum. The postures, including ventral and lateral recumbency to other postures, defecating, urinating, sham-chewing and bar-biting behavior, were observed by video from 07:00 to 09:00 and from 13:00 to 15:00 on the 7th day of each week from the 3rd to the 5th week post-parturition. In addition, the concentrations of salivary interleukin (IL)-6, tumor necrosis factor (TNF)-α and secretory immunoglobulin (SIgA) were assayed after the observed behaviors. The results showed no significant difference between Damin sows and Large White sows in terms of behaviors at the 3rd week. Additionally, there were no significant differences between Damin and Large White sows in terms of the behaviors of ventral recumbency and bar-biting with the exception of lateral recumbency to other postures, sham-chewing, defecation and urination in the fifth week. Meanwhlie, there was significant difference between two breeds in term of ventral recumbency at the 4th week. The result of the ACTH test showed a significant difference between the Damin and Large White sows by the 27th and 34th days postpartum (P<0.01). In addition, the serological concentrations of IL-6 and TNF-α were not significantly different between the two breeds at the 3rd week postpartum. However, these indicators were significantly different at the 5th week postpartum (P = 0.000, and P

Behavior and physiology of two different sow breeds in a farrowing environment during late 35-day lactation

PubMed Central

Wang, Chao; Zhao, Peng; Zhang, Mingyue; Xu, Shiwen; Bao, Jun

2018-01-01

To improve the overall welfare levels of sows and to reduce stress levels at late 35-day lactation, we selected targeted behavioral indicators that might be associated with stress. Therefore, we monitored and evaluated the adaptive capability of two different breeds of sows to the farrowing environment. In this study, Damin sows (Large White × Min pig sows, n = 20) and Large White sows (n = 20) were farrowed in individual pens. Saliva was collected and tested for cortisol density at –15 min, and then at +15, 30, 60, 90, 120, 180 and 240 min after an adrenocorticotropic hormone (ACTH) stimulation test conducted at 20, 27 and 34 d post-partum. The postures, including ventral and lateral recumbency to other postures, defecating, urinating, sham-chewing and bar-biting behavior, were observed by video from 07:00 to 09:00 and from 13:00 to 15:00 on the 7th day of each week from the 3rd to the 5th week post-parturition. In addition, the concentrations of salivary interleukin (IL)-6, tumor necrosis factor (TNF)-α and secretory immunoglobulin (SIgA) were assayed after the observed behaviors. The results showed no significant difference between Damin sows and Large White sows in terms of behaviors at the 3rd week. Additionally, there were no significant differences between Damin and Large White sows in terms of the behaviors of ventral recumbency and bar-biting with the exception of lateral recumbency to other postures, sham-chewing, defecation and urination in the fifth week. Meanwhlie, there was significant difference between two breeds in term of ventral recumbency at the 4th week. The result of the ACTH test showed a significant difference between the Damin and Large White sows by the 27th and 34th days postpartum (P<0.01). In addition, the serological concentrations of IL-6 and TNF-α were not significantly different between the two breeds at the 3rd week postpartum. However, these indicators were significantly different at the 5th week postpartum (P = 0.000, and P

Penetration of chemicals into the oocyte, uterine fluid, and preimplantation blastocyst

PubMed Central

Fabro, Sergio

1978-01-01

Chemicals, including commonly used drugs (e.g., penicillin, meprobamate, pyridium, and mercaptomerin) penetrate and persist for some time in the ovarian follicular fluid at concentrations approximately similar to that of the serum. Information as to the penetration of chemicals into the granulosa cells and into the oocyte is scanty, although there are some indications that these structures are also permeable to foreign chemicals. Similarly, caffeine, nicotine, thiopental, salicylic acid, antipyrine, barbital, and isoniazid enter the uterine secretion and penetrate the preimplantation blastocyst of mice, rats and rabbits. The pattern of distribution of compounds among ovarian follicular fluid, uterine luminal fluid, blastocyst and plasma varies from compound to compound and appears to be related to the molecular weight and degree of ionization of the compound and differs in pregnant and nonpregnant animals. Thus, nicotine and DDT accumulate in the uterine luminal fluid of pregnant but not in that of nonpregnant rabbits. The penetration of foreign chemicals into the oocyte, uterine luminal fluid, and preimplantation blastocyst may exert adverse effects on fertilization, implantation, and/or further development of the conceptus. The possible toxicological importance of this process to eutherian reproduction is discussed. PMID:17539150

Motor and cognitive stereotypies in the BTBR T+tf/J mouse model of autism

PubMed Central

Pearson, BL; Pobbe, RLH; Defensor, EB; Oasay, L; Bolivar, VJ; Blanchard, DC; Blanchard, RJ

2010-01-01

The BTBR T+tf/J inbred mouse strain displays a variety of persistent phenotypic alterations similar to those exhibited in autism spectrum disorders. The unique genetic background of the BTBR strain is thought to underlie its lack of reciprocal social interactions, elevated repetitive self-directed grooming and restricted exploratory behaviors. In order to clarify the existence, range and mechanisms of abnormal repetitive behaviors within BTBR mice, we performed detailed analyses of the microstructure of self-grooming patterns and noted increased overall grooming, higher percentages of interruptions in grooming bouts and a concomitant decrease in the proportion of incorrect sequence transitions compared to C57BL/6J inbred mice. Analyses of active phase home cage behavior also revealed an increase in stereotypic bar-biting behavior in the BTBR strain relative to B6 mice. Finally, in a novel object investigation task, BTBR mice exhibited greater baseline preference for specific unfamiliar objects as well as more patterned sequences of sequential investigations of those items. These results suggest that the repetitive, stereotyped behavior patterns of BTBR mice are relatively pervasive and reflect both motor and cognitive mechanisms. Furthermore, other pre-clinical mouse models of autism spectrum disorders may benefit from these more detailed analyses of stereotypic behavior. PMID:21040460

The detection of drugs of abuse in fingerprints using Raman spectroscopy I: latent fingerprints

NASA Astrophysics Data System (ADS)

Day, Joanna S.; Edwards, Howell G. M.; Dobrowski, Steven A.; Voice, Alison M.

2004-02-01

This paper describes the application of Raman spectroscopy to the detection of exogenous substances in latent fingerprints. The scenario considered was that of an individual handling a substance and subsequently depositing a contaminated fingerprint. Five drugs of abuse (codeine phosphate, cocaine hydrochloride, amphetamine sulphate, barbital and nitrazepam) and five non-controlled substances of similar appearance, which may be used in the adulteration of drugs of abuse (caffeine, aspirin, paracetamol, starch and talc), were studied in both sweat-rich and sebum-rich latent fingerprints. The substances studied could be clearly distinguished using their Raman spectra and were all successfully detected in latent fingerprints. Photobleaching was necessary to reduce the fluorescence background in the spectra of some substances. Raman spectra obtained from the substances in sweat-rich latent fingerprints were of a similar quality to spectra that obtained from the substances under normal sampling conditions. Interfering Raman bands arising from latent fingerprint material were present in the spectra obtained from the substances in sebum-rich fingerprints. These bands did not prevent identification of the substances and could be successfully removed by spectral subtraction. The most difficult aspect of the detection of these substances in latent fingerprints was visually locating the substance in the fingerprint in order to obtain a Raman spectrum.

The history of barbiturates a century after their clinical introduction

PubMed Central

López-Muñoz, Francisco; Ucha-Udabe, Ronaldo; Alamo, Cecilio

2005-01-01

The present work offers an analysis of the historical development of the discovery and use of barbiturates in the field of psychiatry and neurology, a century after their clinical introduction. Beginning with the synthesis of malonylurea by von Baeyer in 1864, and up to the decline of barbiturate therapy in the 1960s, it describes the discovery of the sedative properties of barbital, by von Mering and Fischer (1903), the subsequent synthesis of phenobarbital by this same group (1911), and the gradual clinical incorporation of different barbiturates (butobarbital, amobarbital, secobarbital, pentobarbital, thiopental, etc). We describe the role played in therapy by barbiturates throughout their history: their traditional use as sedative and hypnotic agents, their use with schizophrenic patients in so-called “sleep cures” (Klaesi, Cloetta), the discovery of the antiepileptic properties of phenobarbital (Hauptmann) and their use in the treatment of epilepsy, and the introduction of thiobarbiturates in intravenous anesthesia (Lundy, Waters). We also analyze, from the historical perspective, the problems of safety (phenomena of dependence and death by overdose) which, accompanied by the introduction of a range of psychoactive drugs in the 1950s, brought an end to barbiturate use, except in specific applications, such as the induction of anesthesia and the treatment of certain types of epileptic crisis. PMID:18568113

Rapid and on-site analysis of illegal drugs on the nano-microscale using a deep ultraviolet-visible reflected optical fiber sensor.

PubMed

Li, Qiang; Qiu, Tian; Hao, Hongxia; Zhou, Hong; Wang, Tongzhou; Zhang, Ye; Li, Xin; Huang, Guoliang; Cheng, Jing

2012-04-07

A deep ultraviolet-visible (DUV-Vis) reflected optical fiber sensor was developed for use in a simple spectrophotometric detection system to detect the absorption of various illegal drugs at wavelengths between 180 and 800 nm. Quantitative analyses performed using the sensor revealed a high specificity and sensitivity for drug detection at a wavelength of approximately 200 nm. Using a double-absorption optical path length, extremely small sample volumes were used (32 to 160 nL), which allowed the use of minimal amounts of samples. A portable spectrophotometric system was established based on our optical fiber sensor for the on-site determination and quantitative analysis of common illegal drugs, such as 3,4-methylenedioxymethamphetamine (MDMA), ketamine hydrochloride, cocaine hydrochloride, diazepam, phenobarbital, and barbital. By analyzing the absorbance spectra, six different drugs were quantified at concentrations that ranged from 0.1 to 1000 μg mL(-1) (16 pg-0.16 μg). A novel Matching Algorithm of Spectra Space (MASS) was used to accurately distinguish between each drug in a mixture. As an important supplement to traditional methods, such as mass spectrometry or chromatography, our optical fiber sensor offers rapid and low-cost on-site detection using trace amounts of sample. This rapid and accurate analytical method has wide-ranging applications in forensic science, law enforcement, and medicine.

Quantitative detection of type A staphylococcal enterotoxin by Laurell electroimmunodiffusion.

PubMed

Gasper, E; Heimsch, R C; Anderson, A W

1973-03-01

The detection of staphylococcal enterotoxin A by the quantitative technique of electroimmunodiffusion is described. High dilutions of type-specific rabbit antiserum were used in 1% agarose gels, 1 mm thick, and prepared in 0.05-mug barbital buffer, pH 8.6. Volumes of 10 muliters containing 1.5 to 10 ng of toxin were electrophoresed out of 4-mm diameter wells at 5 mA/cm width of gel. The precipitin cones formed were made visible by first immersing the agarose gels in 0.2 M NaCl and then overlaying the surface with the purified globulin fraction of sheep serum against rabbit globulin, followed by soaking of the gels in 1% aqueous cadmium acetate and staining with 0.1% thiazine red in 1% glacial acetic acid. Fully extended cones, 4 to 23 mm in length depending on toxin concentration and antiserum dilution, were developed in 2 to 5 h of electrophoresis, and visualization was achieved within 2 to 3 h. Because the method is qualitative, quantitative, simple, rapid, and sensitive, it offers a practical tool for the detection of small amounts of bacterial toxins in contaminated foods. The method should also qualify as a sensitive detection device in biochemical procedures which attempt to trace, detect, and identify biological substances in nanogram quantities, provided these substances are antigenic and capable of forming a precipitate with their specific antibodies.

Motor and cognitive stereotypies in the BTBR T+tf/J mouse model of autism.

PubMed

Pearson, B L; Pobbe, R L H; Defensor, E B; Oasay, L; Bolivar, V J; Blanchard, D C; Blanchard, R J

2011-03-01

The BTBR T+tf/J inbred mouse strain displays a variety of persistent phenotypic alterations similar to those exhibited in autism spectrum disorders (ASDs). The unique genetic background of the BTBR strain is thought to underlie its lack of reciprocal social interactions, elevated repetitive self-directed grooming, and restricted exploratory behaviors. In order to clarify the existence, range, and mechanisms of abnormal repetitive behaviors within BTBR mice, we performed detailed analyses of the microstructure of self-grooming patterns and noted increased overall grooming, higher percentages of interruptions in grooming bouts and a concomitant decrease in the proportion of incorrect sequence transitions compared to C57BL/6J inbred mice. Analyses of active phase home-cage behavior also revealed an increase in stereotypic bar-biting behavior in the BTBR strain relative to B6 mice. Finally, in a novel object investigation task, the BTBR mice exhibited greater baseline preference for specific unfamiliar objects as well as more patterned sequences of sequential investigations of those items. These results suggest that the repetitive, stereotyped behavior patterns of BTBR mice are relatively pervasive and reflect both motor and cognitive mechanisms. Furthermore, other pre-clinical mouse models of ASDs may benefit from these more detailed analyses of stereotypic behavior. © 2010 The Authors. Genes, Brain and Behavior © 2010 Blackwell Publishing Ltd and International Behavioural and Neural Genetics Society.

Stability of thiopental and pentobarbital in human plasma determined with a new easy and specific gas chromatography-mass spectrometry assay.

PubMed

Martens-Lobenhoffer, J

1999-08-01

A gas chromatographic-mass spectrometric (GC-MS) assay for the determination of thiopental and its main metabolite pentobarbital in human plasma is presented in this study. The sample preparation consists only in the addition of the internal standard barbital and an acidic extraction with ethyl acetate. Analytical separation is accomplished on a RTX-1 15 m x 0.25 mm capillary column with a film thickness of 0.5 micron. The effluent is observed by a mass selective detector operating in the single ion monitoring mode. The limits of detection are 5 ng/ml for pentobarbital and 10 ng/ml for thiopental, the intra-day variabilities are 2.2% and 4.0% and the inter-day variabilities are 3.3% and 7.1% at concentrations of 5 micrograms/ml, respectively. Applying this assay, the stability of thiopental and pentobarbital in human plasma was tested at concentrations of 5 micrograms/ml each. Thiopental is stable in human plasma at least over 41 days stored at -20 degrees C and 5 degrees C, respectively. A decay of about 2%/day is observed under storage at ambient temperature (19-20 degrees C). Pentobarbital is stable under all storage conditions. Methanolic solutions of thiopental are stable for 83 days under storage at 5 degrees C. Aqueous solutions of thiopental-sodium are stable for at least 23 days under storage at 5 degrees C or ambient temperature.

Simultaneous analysis by Quadrupole-Orbitrap mass spectrometry and UHPLC-MS/MS for the determination of sedative-hypnotics and sleep inducers in adulterated products.

PubMed

Lee, Ji Hyun; Park, Han Na; Choi, Ji Yeon; Kim, Nam Sook; Park, Hyung-Joon; Park, Seong Soo; Baek, Sun Young

2017-12-01

Adulterated products are continuously detected in society and cause problems. In this study, we developed and validated a method for determining synthetic sedative-hypnotics and sleep inducers, including barbital, benzodiazepam, zolpidem, and first-generation antihistamines, in adulterated products using Quadrupole-Orbitrap mass spectrometry and ultrahigh performance liquid chromatography with tandem mass spectrometry. In Quadrupole-Orbitrap mass spectrometry analysis, target compounds were confirmed using a combination of retention time, mass tolerance, mass accuracy, and fragment ions. For quantification, several validation parameters were employed using ultrahigh performance liquid chromatography with tandem mass spectrometry. The limit of detection and limit of quantitation was 0.05-53 and 0.17-177 ng/mL, respectively. The correlation coefficient for linearity was more than 0.995. The intra- and interassay accuracies were 86-110 and 84-111%, respectively. Their precision values were evaluated as within 4.0 (intraday) and 10.7% (interday). Mean recoveries of target compounds in adulterated products ranged from 85 to 116%. The relative standard deviation of stability was less than 10.7% at 4°C for 48 h. The 144 adulterated products obtained over 3 years (2014-2016) from online and in-person vendors were tested using established methods. After rapidly screening with Quadrupole-Orbitrap mass spectrometry, the detected samples were quantified using ultrahigh performance liquid chromatography with tandem mass spectrometry. Two of them were adulterated with phenobarbital. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison between micellar liquid chromatography and capillary zone electrophoresis for the determination of hydrophobic basic drugs in pharmaceutical preparations.

PubMed

Torres-Cartas, S; Martín-Biosca, Y; Sagrado, S; Villanueva-Camañas, R M; Medina-Hernández, M J

2007-01-01

The determination of highly hydrophobic basic compounds by means of conventional reversed-phase liquid chromatographic methods has several drawbacks. Owing to the characteristics of micellar liquid chromatography (MLC) and capillary electrophoresis (CE), these techniques could be advantageous alternatives to reversed-phase chromatographic methods for the determination of these kinds of compounds. The objective of this study was to develop and compare MLC and CE methods for the determination of antipsychotic basic drugs (amitryptiline, haloperidol, perphenazine and thioridazine) in pharmaceutical preparations. The chromatographic determination of the analytes was performed on a Kromasil C(18) analytical column; the mobile phase was 0.04 m cetyltrimethylammonium bromide (CTAB), at pH 3, containing 5% 1-butanol, at a flow rate of 1 mL/min. The CE separation was performed in a fused-silica capillary with a 50 mm tris-(hydroxymethyl)-aminomethane buffer, pH 7, at an applied voltage of 20 kV, using barbital as internal stardard. The proposed methods are suitable for a reliable quantitation of these compounds in the commercial tablets and drops in terms of accuracy and precision and require a very simple pre-treatment of the samples. By comparing the performance characteristics and experimental details of the MLC and CE methods we conclude that CE seems to be slightly better than MLC in the determination of highly hydrophobic compounds in pharmaceuticals in terms of resolution and economy, taking into account that the limits of detection are not a handicap in pharmaceutical samples. Copyright 2006 John Wiley & Sons, Ltd.

The detection of drugs of abuse in fingerprints using Raman spectroscopy II: cyanoacrylate-fumed fingerprints

NASA Astrophysics Data System (ADS)

Day, Joanna S.; Edwards, Howell G. M.; Dobrowski, Steven A.; Voice, Alison M.

2004-07-01

This paper describes the application of Raman spectroscopy to the detection of exogenous substances in cyanoacrylate-fumed fingerprints. The scenario considered was that of an individual handling a substance and subsequently depositing a contaminated fingerprint. These fingerprints were enhanced by cyanoacrylate fuming, a process in which a layer of white cyanoacrylate polymer is deposited on the fingerprint material, enabling visual detection. Five drugs of abuse (codeine phosphate, cocaine hydrochloride, amphetamine sulphate, barbital and nitrazepam) and five non-controlled substances of similar appearance, which may be used in the adulteration of drugs of abuse (caffeine, aspirin, paracetamol, starch and talc), were used. The substances studied could be clearly distinguished using their Raman spectra and were all successfully detected in cyanoacrylate-fumed fingerprints. Photobleaching was necessary to reduce the fluorescence background in the spectra of some substances. Raman spectra obtained from the substances in cyanoacrylate-fumed fingerprints were of a similar quality to spectra obtained from the substances under normal sampling conditions, however, interfering Raman bands arising from the cyanoacrylate polymer were present in the spectra. In most cases the only interfering band was the CN stretching mode of the polymer, and there were no cases where the interfering bands prevented identification of the substances. If necessary, the interfering bands could be successfully removed by spectral subtraction. The most difficult aspect of the detection of these substances in cyanoacrylate-fumed fingerprints was visually locating the substance in the fingerprint beneath the polymer layer in order to obtain a Raman spectrum.