Detection and determination of common benzodiazepines and their metabolites in blood samples of forensic science interest

1988 ◽  
Vol 449 ◽  
pp. 281-297 ◽  
Author(s):  
J.B.F. Lloyd ◽  
D.A. Parry
Keyword(s):  
Forensic Science ◽  
Blood Samples ◽  
Science Interest

A Rapid Method for Determination of Buprenorphine and Norbuprenorphine in Urine by UPLC-MS/MS

2020 ◽  
Vol 16 ◽  
Author(s):  
Aykut Kul ◽  
Murat Ozdemir ◽  
Selma Ozilhan ◽  
Olcay Sagirli
Keyword(s):  
Forensic Science ◽  
Rapid Method ◽  
Proficiency Testing ◽  
Mass Spectrometer ◽  
Illicit Market ◽  
Analysis Methods ◽  
Accuracy And Precision ◽  
Lower Limits

Background: Buprenorphine is quite common in the illicit market. Buprenorphine-containing drugs abuse is frequently encountered in patients. The analysis methods used to determine the abuse of buprenorphine and norbuprenorphine are important for forensic science. Buprenorphine is metabolized to norbuprenorphine by the liver. Objective: Therefore, the determination of buprenorphine and norbuprenorphine in urine is one of the methods to determine the abuse of buprenorphine. Methods: In this study, we have developed a precise, simple, and rapid ultra-performance liquid chromatographytandem mass spectrometer method for the determination of buprenorphine and norbuprenorphine simultaneously. Results: The developed method was validated in terms of selectivity and linearity, which was in the range of 9–1800 ng/mL for both buprenorphine and norbuprenorphine. The intra-assay and inter-assay accuracy and precision were found within acceptable limits of the EMA guideline. Lower limits of quantitation were 9 ng/mL for both buprenorphine and norbuprenorphine. Conclusion: The developed method was successfully applied for the determination of both analytes in the proficiency testing samples.

Synthesis and solvatochromic studies of 2- amino-3-phenolazo1-(4-sulfophenyl)-3-methyi-5-pyrozolone and use it for the determination of trace amount of Nickel (II) in blood samples

2016 ◽  
Vol 5 (10) ◽  
pp. 4920
Author(s):  
Amar M. Ali ◽  
Hussain. J. Mohammed*
Keyword(s):  
Stability Constant ◽  
Trace Amount ◽  
Benzenesulfonic Acid ◽  
Determination Method ◽  
Blood Samples ◽  
Determination Of Nickel ◽  
Normal Human ◽  
The Stability ◽  
Normal Human Blood

A new, simple, sensitive and rapid spectrophotometric method is proposed for the determination of trace amount of Nickel (II). The method is based on the formation of a 1:2 complex with 4-(4-((2-hydroxy-6-nitrophenyl) diazenyl) -3-methyl-5-oxo-2, 5-dihydro-1H-pyrazol-1-yl) benzenesulfonic acid (2-ANASP) as a new reagent is developed. The complex has a maximum absorption at 516 nm and εmax of 1. 84 X 105 L. mol-1. cm-1. A linear correlation (0. 25 – 4. 0μg. ml-1) was found between absorbance at λmax and concentration. The accuracy and reproducibility of the determination method for various known amounts of Nickel (II) were tested. The results obtained are both precise (RSD was 1. 2 %) and accurate (relative error was 0. 787 %). The effect of diverse ions on the determination of Nickel (II) to investigate the selectivity of the method were also studied. The stability constant of the product was 0. 399 X 106 L. mol-1. The proposed method was successfully applied to the analysis of diabetes blood and normal human blood. 

scholarly journals Determination of 19 Psychoactive Substances in Premortem and Postmortem Whole Blood Samples Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry

Separations ◽  
2021 ◽  
Vol 8 (6) ◽  
pp. 78
Author(s):  
Sevasti Karampela ◽  
Jessica Smith ◽  
Irene Panderi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
Whole Blood ◽  
High Performance ◽  
Tandem Mass ◽  
Psychoactive Substances ◽  
Blood Samples ◽  
Whole Blood Samples

An ever-increasing need exists within the forensic laboratories to develop analytical processes for the qualitative and quantitative determination of a broad spectrum of new psychoactive substances. Phenylethylamine derivatives are among the major classes of psychoactive substances available on the global market and include both amphetamine analogues and synthetic cathinones. In this work, an ultra-high-performance liquid chromatography-positive ion electrospray ionization tandem mass spectrometric method (UHPLC-ESI-MS/MS) has been developed and fully validated for the determination of 19 psychoactive substances, including nine amphetamine-type stimulants and 10 synthetic cathinone derivatives, in premortem and postmortem whole blood. The assay was based on the use of 1 mL premortem or postmortem whole blood, following solid phase extraction prior to the analysis. The separation was achieved on a Poroshell 120 EC-C18 analytical column with a gradient mobile phase of 0.1% formic acid in acetonitrile and 0.1% formic acid in water in 9 min. The dynamic multiple reaction monitoring used in this work allowed for limit of detection (LOD) and lower limit of quantitation (LOQ) values of 0.5 and 2 ng mL−1, respectively, for all analytes both in premortem and postmortem whole blood samples. A quadratic calibration model was used for the 12 quantitative analytes over the concentration range of 20–2000 ng mL−1, and the method was shown to be precise and accurate both in premortem and postmortem whole blood. The method was applied to the analysis of real cases and proved to be a valuable tool in forensic and clinical toxicology.

LRF and TRF test during long-term danazol treatment: increase of the LH and FSH responses but decrease of the prolactin and TSH responses

1983 ◽  
Vol 104 (1) ◽  
pp. 1-5 ◽  
Author(s):  
J. Leppäluoto ◽  
L. Rönnberg ◽  
P. Ylöstalo
Keyword(s):  
Clinical Symptoms ◽  
Follicular Phase ◽  
Blood Samples ◽  
Hormone Levels ◽  
Coefficients Of Variation ◽  
The Mean ◽  
Thyroid Hormone Levels ◽  
Low Serum

Abstract. Seven patients suffering from severe endometriosis were treated with danazol 200 mg × 3 daily for 6 months. Clinical symptoms were alleviated and menses disappeared in response to the treatment. After cessation of the treatment the menstrual bleedings returned in 1–3 months. Blood samples for determination of gonadotrophins, prolactin (Prl), oestradiol (E2), progesterone, thyroid hormones and thyrotrophin in radioimmunoassays were taken and a combined TRF and LRF test carried out in the follicular phase before treatment, at the 6th month of treatment and after reappearance of the first menses. There were no statistically significant changes in the basal levels of serum FSH, LH or TSH during the danazol treatment. Neither was there any change in episodic secretions of FSH, LH or Prl, as determined by the mean coefficients of variation of the hormone levels in seven consecutive samples taken at 20 min intervals. On the other hand, serum E2, Prl and thyroid hormone levels were significantly decreased in the 6th month of treatment. In the TRF-LRF test the responses of serum FSH and LH were significantly higher and those of serum Prl and TSH significantly lower during danazol treatment than before. Prl responses remained lowered after the treatment. It appears that low serum oestrogen levels, induced by the danazol treatment, sensitize the pituitary gonadotrophs to exogenous LRF, but make the sensitivity of thyrotrophs and lactotrophs lower to exogenous TRF. These results thus indicate that danazol does not make the pituitary gonadotrophs insensitive to LRF, but danazol may rather inhibit the secretion of hypothalamic LRF.

scholarly journals Simultaneous Determination of Cyclosporine A, Tacrolimus, Sirolimus, and Everolimus in Whole-Blood Samples by LC-MS/MS

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Mustafa Karapirli ◽  
Murat Kizilgun ◽  
Ozgur Yesilyurt ◽  
Husamettin Gul ◽  
Zeki Ilker Kunak ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Cyclosporine A ◽  
Whole Blood ◽  
Immunosuppressive Drugs ◽  
Tandem Mass ◽  
Blood Samples ◽  
Whole Blood Samples

Objectives. Cyclosporine A (CyA), tacrolimus (TRL), sirolimus (SIR), and everolimus (RAD) are immunosuppressive drugs frequently used in organ transplantation. Our aim was to confirm a robust sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination of CyA, TRL, SIR, and RAD in whole-blood samples.Materials and Methods. We used an integrated online solid-phase extraction-LC-MS/MS system and atmospheric pressure ionization tandem mass spectrometry (API-MS/MS) in the multiple reaction monitoring (MRM) detection mode. CyA, TRL, SIR, and RAD were simultaneously analyzed in whole blood treated with precipitation reagent taken from transplant patients.Results. System performance parameters were suitable for using this method as a high-throughput technique in clinical practice. The high concentration of one analyte in the sample did not affect the concentration of other analytes. Total analytical time was 2.5 min, and retention times of all analytes were shorter than 2 minutes.Conclusion. This LC-MS/MS method can be preferable for therapeutic drug monitoring of these immunosuppressive drugs (CyA, TRL, SRL, and RAD) in whole blood. Sample preparation was too short and simple in this method, and it permits robust, rapid, sensitive, selective, and simultaneous determination of these drugs.

Rapid and reliable determination of the halogenating peroxidase activity in blood samples

2014 ◽  
Vol 415 ◽  
pp. 46-56 ◽  
Author(s):  
Jörg Flemmig ◽  
Pauline Schwarz ◽  
Ingo Bäcker ◽  
Anna Leichsenring ◽  
Franziska Lange ◽  
...  
Keyword(s):  
Peroxidase Activity ◽  
Reliable Determination ◽  
Blood Samples

scholarly journals Effects of Delayed Sample Processing on Determination of Total and High Molecular Weight (HMW) Adiponectin in Serum and Plasma: A Pilot Study

2016 ◽  
Vol 8 (3) ◽  
pp. 19
Author(s):  
Choaping Ng ◽  
Felicity J Rose ◽  
Sahar Keshvari ◽  
Marina M Reeves ◽  
Goce Dimeski ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Pilot Study ◽  
High Molecular Weight ◽  
Accurate Determination ◽  
Mean Difference ◽  
Serum Samples ◽  
Blood Samples ◽  
Hmw Adiponectin ◽  
Total Adiponectin

<p>Adiponectin is a beneficial adipocyte-secreted hormone, which circulates in a variety of multimeric forms termed low and high molecular weight (LMW/HMW). Effectiveness of clinical therapeutic trials which target adiponectin rely on accurate determination of circulating total and HMW adiponectin levels but the accuracy may be influenced by variations in sample handling processes. The aim of this pilot study was to investigate the effects of delayed processing of blood samples on the concentration of total and HMW adiponectin.</p><p>Materials and Methods: Fasting blood samples were collected for analysis of total and HMW adiponectin concentrations in EDTA plasma and serum from eight healthy participants.  Samples were centrifuged post 15 min storage at 4<sup>o</sup>C as the comparative ‘ideal’ method or after up to 72 h of refrigerated storage or 6 h at room temperature. Total and HMW adiponectin concentrations were measured by ELISA.</p><p>Results: Under ideal handling conditions measurements of total and HMW adiponectin concentrations were significantly higher in serum than in plasma (mean difference: -1.3 µg/mL [95% CI: -1.6, -1.0], p&lt;0.001; and, -0.6 µg/mL [95% CI: -0.7, -0.5], p&lt;0.001, respectively).  Storage of blood samples at 4<sup>o</sup>C for 72 h resulted in significant reductions in concentration of total adiponectin in serum (mean difference: -1.4 µg/mL [95% CI: -2.0, -0.8], p=0.001) and HMW adiponectin in plasma (mean difference: -0.6 µg/mL [95%CI: -0.9, -0.2], p=0.007), compared with ideal conditions.  Further analysis of serum samples showed a significant decrease in total adiponectin concentration after 6 h storage at 4<sup>o</sup>C (mean difference: -1.4 µg/mL [95% CI: -2.0, -0.8], p=0.001) compared with ideal conditions.</p><p>Conclusions: Delayed processing of samples may have differential effects on the concentration of total and HMW adiponectin in serum or plasma. Larger studies are warranted for clinical intervention trials.</p>

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