MICROCHEMICAL JOURNAL
·
2023
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IF 4.8
Yanshuxian Liu,Yilei Fan,Yin Zheng,Zhongping Huang,Huijun Liu,Zhenlu Shen,Yu Xu,Danxia Yu,Xuedong Xiao
A sensitive and novel method for the determination of methamphetamine (MAMP), 3,4-methylenedioxymethamphetamine (MDMA) and their metabolites amphetamine (AMP), 3,4-methylenedioxyamphetamine (MDA) in human hair was established by the employment of flash evaporation-gas chromatography/mass spectrometry (FE-GC/MS) combined with micro-reaction device. 0.30 mg human hair after cutting was put into a sealed glass capillary and heated at 270 °C in a pyrolyzer for 0.5 min. MAMP, AMP, MDMA and MDA evaporated from the hair were converted into their corresponding trifluoroacetylation product in a 60 °C water bath for 30 min with the acetylation by 2 μL trifluoroacetic anhydride (TFAH). Thus, amphetamines (AMPs) in human hair were separated and detected by GC/MS in SIM mode. The obtained calibration curves showed good linearity with the concentrations of MAMP, MDMA and MDA at 1–100 ng/mg, and AMP at 2–100 ng/mg. The linear correlation coefficients (r) were all larger than 0.996. Limits of detection for MAMP, AMP, MDMA and MDA were 0.67, 0.07, 0.17 and 0.07 ng/mg respectively. Limits of quantification for MAMP, AMP, MDMA and MDA were 2.00, 0.20, 0.50 and 0.20 ng/mg respectively. The precision over a range of 0.63–9.98 % were obtained with the recoveries of 92.7–115.2 % for AMPs. Five positive hair samples, three suspicious hair samples and two negative hair samples were successfully analyzed. The results of FE-GC/MS with micro-reaction device were comparable with those found by the referenced method. It was demonstrated that the developed method had potential applications for the analysis of AMPs in hair.
研究领域:
毒理学
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分析化学
✓ 已验证
产品关联
DOI
高影响因子
Forensic Toxicology
·
2022
·Vol. 40
·期 2
·312-321
·
IF 2.541
Ji Jiao-jiao,Zhao Junbo,Xiang Ping,Yan Hui,Shen Min
Purpose Methorphan exists in two enantiomeric forms including dextromethorphan and levomethorphan. Dextromethorphan is an over-the-counter antitussive drug, whereas levomethorphan is strictly controlled as a narcotic drug. Chiral analysis of methorphan could, therefore, assist clinicians and forensic experts in differentiating between illicit and therapeutic use and in tracing the source of the drug. Methods A method for enantiomeric separation and quantification of levomethorphan and dextromethorphan in human hair was developed and validated using liquid chromatography–tandem mass spectrometry (LC–MS/MS). Hair was extracted in hydrochloric acid/methanol (1:20, v/v). The supernatant were separated using a Supelco Astec Chirobiotic™ V2 column (250 × 2.1 mm, i.d., 5 μm particle size) and analyzed on a triple quadrupole linear ion trap mass spectrometer in multiple reaction monitoring mode. Results The limits of detection for dextromethorphan and levomethorphan were 2 and 1 pg/mg, respectively; the lower limit of quantification was 2 pg/mg for both drugs. Good linearity ( r > 0.995) was observed for both analytes over the linear range. Precision values were below 10% for both analytes; accuracy values ranged from 87.5 to 101%. The extraction recoveries were 78.3–98.4%, and matrix effects were 70.5–88.6%. This method was applied to human hair samples from 120 people suspected of methorphan use to further distinguish the drug chirality. Dextromethorphan was detected in all 120 samples at a concentration range of 2.7–19,100 pg/mg, whereas levomethorphan was not detected in any sample. Conclusions A sensitive quantitative method was established for the enantiomeric separation of dextromethorphan and levomethorphan in hair. This is the first study to achieve chiral analysis of methorphan in human hair.
研究领域:
法医学
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药物分析
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临床毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
·
2025
·
IF 1.3
Aiying SONG,Rong LIU,Xinghe HE,Linlin WEI
In the field of forensic sciences, the analysis of amphetamine-type stimulants in hair samples has become a fundamental tool for assessing long-term substance use. The persistent nature of amphetamine-type stimulants in hair provides a unique chronological record of drug intake, offering valuable insights for legal and clinical applications. Developing a simple, sensitive, and reliable method for the determination of these drugs in hair samples remains an important issue in forensic analysis. In this study, polydimethylsiloxane modified stainless steel fiber was firstly fabricated. By taking advantage of the affinity of the polydimethylsiloxane coating toward amphetamine-type stimulants and the excellent conductivity of stainless steel wire, an electro-enhanced solid-phase microextraction coupled with gas chromatography equipped with a nitrogen-phosphorus detector method was established to sensitively determine four common amphetamine-type stimulants in hair samples. The experimental results showed a linear range from 0.1 to 50 µg L⁻¹. The limits of detection and qualification respectively varied from 0.012 to 0.039 and 0.05 to 0.13 µg L⁻¹ ( S / N = 3), and it exhibited good reproducibility (< 6.2%). Recoveries ranging from 79% to 106%, with a relative standard deviation of < 6.7%, were obtained for all analytes. Fiber-to-fiber reproducibility (RSD), obtained using three fibers, was < 8.8%. The developed strategy combined the affinity of the polydimethylsiloxane coating towards amphetamine-type stimulants with the electrical conductivity of the stainless steel wire, effectively improving the enrichment ability and detection sensitivity, and achieving simultaneous selective enrichment and detection of several analytes. This is a simple, efficient, and reliable method for the analysis of amphetamine-type stimulants from complex matrices.
研究领域:
法医学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS
·
2020
·
IF 3.905
Yanshuxian Liu,Yilei Fan,Zhongping Huang,Huijun Liu,Lili Wang,Zhenlu Shen,Ichi Watanabe
A novel method based on on-line pyrolytic methylation-gas chromatography/mass spectrometry was established and applied into rapid determination of γ-hydroxybutyric acid (GHB) in human hair. With the pyrolytic methylation by tetramethylammonium hydroxide (TMAH), GHB was converted into its corresponding methyl ester in the pyrolyzer at 500 °C. Thus, GHB in hair samples could be well determined by GC/MS on a capillary column in SIM mode. To obtain optimum methylation conditions, important factors were investigated and then applied to the following experiments. The results were obtained as following: 500 °C as reaction temperature, 2:1 as the proportion of TMAH to GHB. The achieved calibration curve exhibited good linearity with the correlation coefficient of 0.9997 at the concentraion range of 2−200 ng/mg, and relative standard deviation (n = 3) from 1.3 %–7.7 %. The limit of detection and the limit of quantification were down to 0.3 ng/mg and 1.0 ng/mg, respectively. The precision ranged from 2.0 %–7.9 % and the recovery ranged from 98.5 %–107.4 %. The results of on-line pyrolytic methylation-GC/MS were in agreement with those observed by the referenced off-line silylation-GC/MS method. The method was applied to a real case of a woman addicted to GHB, the drug concentration in hair segments of 0−5 cm and 5−10 cm from the root strand well correlated with the use of GHB in different periods of her life. The proposed method demonstrated significant potential in the application of rapid determination for GHB in human hair.
研究领域:
法医毒理学
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药物代谢
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分析化学
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生物样本分析
·
临床化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）