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    XIANG Ping

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    法医学杂志    2018, 34 (6): 577-584.   DOI: 10.12116/j.issn.1004-5619.2018.06.001
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    Determination of Oleandrin in Blood and Liver Samples by LC-MS/MS
    ZHAI Jin-xiao, YAN Hui, SHEN Min,et al.
    法医学杂志    2018, 34 (6): 585-589.   DOI: 10.12116/j.issn.1004-5619.2018.06.002
    Abstract379)      PDF(pc) (1403KB)(849)       Save
    Objective To develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) analytical method for the determination of oleandrin in blood and liver tissues, which could be applied to the cases of death caused by oleander poisoning. Methods Blood or liver tissues underwent a liquid-liquid extraction (LLE) using ethyl acetate, and the extract was separated on an Agilent ZORBAX SB-C18 column and eluted with a gradient of acetonitrile and 20 mmol/L ammonium acetate (containing 0.1% formic acid). Oleandrin was detected using electrospray positive ionization (ESI+) with multiple-reaction monitoring (MRM) mode. Results Oleandrin showed excellent linearity in both blood and liver samples in the corresponding linear range (r>0.995 0), with detection limits 1 ng/mL and 2 ng/g, respectively, extraction recovery rates greater than 70.50%, both intra- and inter-day precisions less than 10.71%, accuracies 98.42%-111.63%, and matrix effects 91.52%-106.39%. The method was successfully applied to a case of suspected oleander poisoning. Oleandrin was detected in the blood, urine, liver tissues, bile, stomach wall tissues and stomach contents of the cadaver, with the content ranging from 65.5 to 29 600.0 ng/mL (ng/g). Conclusion The method developed in this study is simple and convenient to operate with good selectivity, and is suitable for the analysis of oleandrin in biological samples such as blood and liver tissues, which can provide technical support for forensic identification and clinical diagnosis and treatment of oleander poisoning.
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    Analysis of Common Herbicides in Blood by UPLC-HRMS
    YANG Yang, ZHANG Xiao-guang, YU Feng,et al .
    法医学杂志    2018, 34 (6): 590-594,600.   DOI: 10.12116/j.issn.1004-5619.2018.06.003
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    Objective To develop a method to screen and quantify 10 common herbicides (paraquat, diquat, glyphosate, glufosinate, cyanazine, atrazine, metazachlor, acetochlor, chlorsulfuron, and metsulfuron) in blood. Methods With acetonitrile-water solution [V(acetonitrile)∶V(water)=3∶1] as protein precipitant, 10 common herbicides in blood were detected using ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). Results All the 10 herbicides had good linearity in their linear range (coefficient of determination R2≥0.993), with the recovery rates 67.4%-111.9%, the relative standard deviations 1.5%-10.8%, the accuracies 85.1%-106.1%, intra-day precisions 2.7%-13.5%, and inter-day precisions 3.3%-13.3%. Conclusion This method is easy to operate with high recovery rates. It enables rapid and accurate qualitative screening and quantitative analysis of various herbicides in blood simultaneously.
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    Retention Time of Four Common Poisons (Drugs) by GC-MS Qualitative Analysis
    LIU Shao-dan, MIN Tao, WANG Mei,et al.
    法医学杂志    2018, 34 (6): 595-600.   DOI: 10.12116/j.issn.1004-5619.2018.06.004
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    Objective To investigate the maximum allowable deviation of retention time (RT) or relative retention time (RRT) between the common poisons (drugs) and standard solvent by gas chromatography-mass spectrometry (GC-MS). Methods After pretreatment with liquid-liquid extraction, four common poisons (drugs)—dichlorvos, phorate, diazepam and estazolam—were detected by full scan mode GC-MS. RT and RRT were analyzed according to combined uncertainty and expanded uncertainty. Results The expanded uncertainty of RT and RRT were 6.0×10-4-14.1×10-3 and 2.5×10-6-5.9×10-5 (k=3), respectively. The RT of poisons (drugs) was relatively stable in blood samples with different mass concentrations. Among dichlorvos, phorate, diazepam and estazolam, the absolute deviation and relative deviation of RT were ≤0.03 min and ≤0.4%, respectively, and those of RRT were ≤0.003 min and ≤0.3%, respectively. Conclusion The maximum allowable deviations of RT and RRT for common poisons (drugs) in blood samples are recommended to be ±0.05 min and ±0.5%.
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    Decomposition Kinetics of Omethoate in Blood
    LI Peng, WANG Hao-yu, BI Wen-ji,et al.
    法医学杂志    2018, 34 (6): 601-605,610.   DOI: 10.12116/j.issn.1004-5619.2018.06.005
    Abstract224)      PDF(pc) (1273KB)(616)       Save
    Objective To study the decomposition kinetics of omethoate in blood. Methods The acetonitrile precipitated protein was added into the blood, with the chromatographic column of a Waters BEH C18 column (2.1 mm×50 mm, 1.7 μm), the mobile phase of 5 mmol/L ammonium acetate aqueous solution-methanol, and the gradient elution with a flow rate of 0.3 mL/min and injection volume of 2 μL. With electrospray ionization (ESI) source and positive ion detection, qualitative and quantitative analyses were taken using multi-reaction monitoring mode. Omethoate standard was added into blank human blood to the mass concentrations of 0.78, 1.40, 2.30, 4.50, and 7.20 μg/mL, and each mass concentration was preserved at 3 temperatures of -20 ℃, 4 ℃, and 20 ℃, respectively. The content of omethoate was detected at different time points (0, 1, 3, 4, 7, 11, 15, 24, 32, 40, 48, 64, 80, 96, and 120 d). Results Different concentrations of omethoate all showed a descended trend in human blood under different temperature conditions. The decomposition in storage environment of -20 ℃, 4 ℃, and 20 ℃ was fit to a one-compartment open model with a first-order kinetic process, which could be expressed as Ct=Coe-αt, with the calculated theoretical values of omethoate concentration close to the measured values. Conclusion All concentrations of omethoate are decomposed in the blood, which vary a lot in different preservation conditions. It is suggested that blood samples should be frozen and detected timely in suspected omethoate poisoning cases.
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    Qualitative and Quantitative Analysis of Cathinones in Human Urine by SPE-GC-MS
    WANG Ping, LIU Xiao-yun, LIU Yao,et al
    法医学杂志    2018, 34 (6): 606-610.   DOI: 10.12116/j.issn.1004-5619.2018.06.006
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    Objective To propose an alternative solid phase extraction-gas chromatography-mass spectrometry (SPE-GC-MS) method for the sensitive determination of cathinones in human urine samples, plus methodological verification. Methods Human urine samples were concentrated by solid phase extraction (SPE) sorbent and converted into the corresponding heptafluorobutyric acid anhydride derivatives. Methcathinone, 4-methyl methcathinone and 3,4-methylenedioxy-N-methylcathinone were detected by gas chromatography-mass spectrometry (GC-MS). With quantitative analysis by internal standard method, methodological verification was carried out from the aspects of specificity, precision and reco-very rate. Results Methcathinone, 4-methyl methcathinone and 3,4-methylenedioxy-N-methylcathinone showed good linearly in the range of 25-200 ng/mL of urine (r>0.99), with the limits of detection 2.0 ng/mL, limit of quantitation 25.0 ng/mL, both intra- and inter-day coefficients of variation lower than 6.0%, and recovery rates of 98.4%-105.7%. Conclusion The proposed SPE-GC-MS procedure has good accuracy and specificity, can meet the need of qualitative and quantitative analysis of cathinones in the urine of drug abusers, and  therefore provide technical support for the detection of cathinone abuse.
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    Research Status of New Designer Drug Methcathinone in Forensic Toxicology
    DENG Yan-fei, LIU Liang, YANG Zhi-xi,et al.
    法医学杂志    2018, 34 (6): 611-616.   DOI: 10.12116/j.issn.1004-5619.2018.06.007
    Abstract292)      PDF(pc) (973KB)(808)       Save
    Methcathinone, a new cathinone designer drug, which is structurally similar to amphetamine analogs, is a central nervous stimulant. Recently, there has been a worldwide rise in its popularity and abuse, and a growing number of cases with disability or even death is reported in several countries, resulting in public concern. The typical symptoms include accelerated heartbeat, high temperature, anxiety, depression, etc. Forensic studies on its toxicity mechanism are rare. This article reviews its toxicological effects, poisoning symptoms, poisoning and addiction mechanisms, and detection methods, to provide theoretical reference for future studies and guidance for related forensic identification.
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    法医学杂志    2018, 34 (6): 617-618.   DOI: 10.12116/j.issn.1004-5619.2018.06.008
    Abstract172)      PDF(pc) (880KB)(654)       Save
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