A simple quantitation method for benzoylecgonine from oral fluid, blood, and urine samples used for determining 22 illicit and licit drugs by GC–MS with liquid–liquid extraction

2012 ◽  
Vol 30 (1) ◽  
pp. 59-65 ◽  
Author(s):  
László Institóris ◽  
Vilmos Angyal ◽  
Zsófia Árok ◽  
Éva Kereszty ◽  
Tibor Varga
Author(s):  
Ana Carolina Furiozo Arantes ◽  
Kelly Francisco da Cunha ◽  
Marilia Santoro Cardoso ◽  
Karina Diniz Oliveira ◽  
Jose Luiz Costa

Abstract Purpose We developed and validated a method for quantitative analysis of 50 psychoactive substances and metabolites (antidepressants, benzodiazepines and opioids) in oral fluid samples using simple liquid–liquid extraction procedure followed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). Method Oral fluid samples were collected using Quantisal™ device and extracted by liquid–liquid extraction with 1.0 mL of methyl tert-butyl ether and then analyzed using LC–MS/MS. Results The method attended method validation criteria, with limits of quantification as low as 0.5 and 1.0 ng/mL, and linearity between 0.5–50.0 ng/mL for antidepressants, 0.5–25.0 ng/mL for benzodiazepines and 1.0–50.0 ng/mL to opioids. During method validation, bias and imprecision values were not greater than 16 and 20%, respectively. Ionization suppression/enhancement bias results were not greater than 25%. No evidence of carryover was observed. Sample stability studies showed that almost all analytes were stable at 25 °C for 3 days and at 4 °C for 7 days. Freeze–thaw cycles stability showed that most antidepressants and opioids were stable under these conditions. Autosampler stability study showed that all analytes were stable for 24 h, except for nitrazepam and 7-aminoclonazepam. Thirty-eight authentic oral fluid samples were analyzed; 36.8% of the samples were positive for 2 drugs. Citalopram was the most common drug found, followed by venlafaxine. Conclusions The method was validated according to international recommendations for the 50 analytes, showing low limits of quantification, good imprecision and bias values, using simple liquid–liquid extraction, and was successfully applied to authentic oral fluid samples analysis.


2016 ◽  
Vol 9 (1) ◽  
pp. 30
Author(s):  
Wei Zhang ◽  
Jun Wang ◽  
Zhiyuan Mi ◽  
Jiangtao Su ◽  
Xiangyu You ◽  
...  

Although misuse and abuse of Cannabis is well known, the health benefits have been proved by various biomedical studies. Tetrahydrocannabinol (THC) is the major active substance in leaves of Cannabis, which is the common target for drug testing. In field drug testing, oral fluid (OF) has its unique advantages over other specimens such as blood, urine, and hair. Thus the study of THC in OF is gaining popularity in Cannabis research. In this review, extraction methods are introduced in three categories, which are Liquid-Liquid Extraction (LLE), Solid Phase Extraction (SPE), and Supercritical Fluid Extraction (SFE). Examples of application with each method will be covered. Advantages and disadvantages of these methods will be compared. In addition, methods in analysis following extraction will be briefly discussed.


2015 ◽  
Vol 1384 ◽  
pp. 1-8 ◽  
Author(s):  
Sergio Armenta ◽  
Salvador Garrigues ◽  
Miguel de la Guardia ◽  
Judit Brassier ◽  
Manel Alcalà ◽  
...  

Author(s):  
Ahmad Shekari ◽  
Rooholah Valipour ◽  
Mehrdad Setareh ◽  
Kambiz Soltaninejad

Background: Methadone abuse and dependence has been reported as a growing concern in some countries. In present study, a rapid, simple, easy and sensitive method for determination of methadone in human urine samples for use in clinical and forensic toxicology and drug screening laboratories was developed and validated. Methods: We determined methadone in urine sampled by gas chromatography/mass spectrometry (GC/MS) and used ultrasound assisted liquid-liquid extraction (UALLE) method for the extraction and preconcentration of methadone before analysis. Results: The limit of detection was 2.1 ng/mL and the limit of quantification 7 ng/mL. Correlation coefficient was 0.9984 for the methadone calibration curve in linear range from 7 to 10,000 ng/mL. The method is accurate and precise. Recovery was in the range of  81.3 % to 97.4 % and enrichment factor was 8.7. The method was successfully applied for determining methadone in clinical and postmortem urine samples. Conclusions: The present method is a rapid, simple, easy and sensitive procedure and can be used in clinical and forensic toxicology laboratories as routine method for qualitative and quantitative analysis of methadone.  


2016 ◽  
Vol 36 (2) ◽  
pp. 195-202 ◽  
Author(s):  
L Bahmanabadi ◽  
M Akhgari ◽  
F Jokar ◽  
HB Sadeghi

Methamphetamine abuse is one of the most medical and social problems many countries face. In spite of the ban on the use of methamphetamine, it is widely available in Iran’s drug black market. There are many analytical methods for the detection of methamphetamine in biological specimen. Oral fluid has become a popular specimen to test for the presence of methamphetamine. The purpose of the present study was to develop a method for the extraction and detection of methamphetamine in oral fluid samples using liquid–liquid extraction (LLE) and gas chromatography/mass spectrometry (GC/MS) methods. An analytical study was designed in that blank and 50 authentic oral fluid samples were collected to be first extracted by LLE and subsequently analysed by GC/MS. The method was fully validated and showed an excellent intra- and inter-assay precision (reflex sympathetic dystrophy ˂ 10%) for external quality control samples. Recovery with LLE methods was 96%. Limit of detection and limit of quantitation were 5 and 15 ng/mL, respectively. The method showed high selectivity, no additional peak due to interfering substances in samples was observed. The introduced method was sensitive, accurate and precise enough for the extraction of methamphetamine from oral fluid samples in forensic toxicology laboratories.


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