1.Research Progress on Biological Matrix Reference Materials in Forensic Toxicology.
Hang CHEN ; Jing HU ; Zheng QIAO ; Hong-Xiao DENG ; Min LÜ ; Wei LIU
Journal of Forensic Medicine 2023;39(2):176-185
Biological matrix reference material is a reference material that combines the target material with the biological matrix. The biological matrix reference material has higher consistency with the authentic specimens in forensic toxicology, and its application has a positive effect on improving the accuracy of test results. This paper reviews the research on the matrix reference materials corresponding to three common biological test materials (blood, urine and hair). In order to provide reference for the development and application of biological matrix reference materials in forensic toxicology, this paper mainly introduces the research progress of preparation technology of biological matrix reference materials and some existing products and their parameters evaluation.
Forensic Toxicology/methods*
;
Hair
;
Body Fluids
2.Development and Application of Metabonomics in Forensic Toxicology.
Journal of Forensic Medicine 2015;31(3):219-226
Metabonomics is an important branch of system biology following the development of genomics, transcriptomics and proteomics. It can perform high-throughput detection and data processing with multiple parameters, potentially enabling the identification and quantification of all small metabolites in a biological system. It can be used to provide comprehensive information on the toxicity effects, toxicological mechanisms and biomarkers, sensitively finding the unusual metabolic changes caused by poison. This article mainly reviews application of metabonomics in toxicological studies of abused drugs, pesticides, poisonous plants and poisonous animals, and also illustrates the new direction of forensic toxicology research.
Animals
;
Biomarkers
;
Forensic Toxicology/methods*
;
Humans
;
Metabolomics/methods*
3.Detection and application of ethyl glucuronide in forensic toxicology.
Hui ZHAO ; Xian-yi ZHUO ; Bao-hua SHEN
Journal of Forensic Medicine 2009;25(1):63-67
Ethyl glucuronide is a specific metabolite of ethanol. There have been plenty of articles referring its pharmacokinetics, detection and application as a specific bio-marker of alcohol intake. This article reviews various analytical methods of EtG, relationship between EtG quantification and ethanol intake, and criteria for determining chronic alcohol abuse, and origin of ethanol found in the cadavers by EtG analysis. EtG has its potential application in forensic toxicology.
Alcoholism/metabolism*
;
Forensic Toxicology/methods*
;
Glucuronates/urine*
;
Hair/chemistry*
;
Humans
4.Measurement of acetonitrile in blood and urine by head-space gas chromatography.
Ru-Xin LUO ; Xian-Yi ZHUO ; Bao-Hua SHEN
Journal of Forensic Medicine 2012;28(6):422-425
OBJECTIVE:
To establish the method for measurement of acetonitrile in blood and urine by head-space gas chromatography.
METHODS:
DB-ALC1 (30 m x 320 microm x 1.8 microm) and DB-ALC2 (30 m x 320 microm x 1.2 microm) capillary column were used to measure the acetonitrile in blood and urine with the isopropanol as internal standard reference.
RESULTS:
The limits of detection of acetonitrile in both blood and urine were 0.5 microg/mL, with a linear range of 5-1000 microg/mL (r = 0.999).The accuracy of this method was 93.2%-98.0%. The RSD for the intra-day and inter-day were less than 3.7%.
CONCLUSION
The method is capable for measurement analysis of acetonitrile in blood and urine.
Acetonitriles/urine*
;
Chromatography, Gas/methods*
;
Cyanides/urine*
;
Forensic Toxicology/methods*
;
Humans
;
Reproducibility of Results
;
Suicide, Attempted
5.How to validate a bio-analytical method.
Ping XIANG ; Min SHEN ; Xian-Yi ZHUO
Journal of Forensic Medicine 2008;24(1):60-65
It is imperative that any newly established bio-analytical method is validated thoroughly, using standardised parameters. The purpose of this article is to provide recommendations on how to validate a new bio-analytical method. Based on author's personal experience and some interesting discussion points from the conference of "International Association of Forensic Toxicologists" in 2007, the authors propose these essential requirements for validating a new analytical method. The key parameters of method validation include selectivity, linearity, accuracy, precision, LOD (limit of detection), LLOQ (the lower limit of quantitation), stability and the extraction recovery. For any bio-analytical method using LC-MSn (Liquid chromatography-mass spectrometry), studies of matrix effect should also be included in addition of the above parameters.
Chemistry Techniques, Analytical/standards*
;
Chromatography, Liquid/methods*
;
Forensic Toxicology
;
Mass Spectrometry/methods*
;
Reproducibility of Results
;
Validation Studies as Topic
6.Simultaneous analyses of cocaine and its metabolite benzoylecgonine in urine by LC-MS/MS.
Qi-ran SUN ; Ping XIANG ; Hui YAN ; Min SHEN
Journal of Forensic Medicine 2008;24(4):268-272
OBJECTIVE:
To establish a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous analysis of cocaine (COC) and its metabolite benzoylecgonine(BZE) in urine samples.
METHODS:
A single dose of COC (10 mg/kg) was injected intraperitoneally into guinea pigs and urine samples were collected for 7 days. The urine samples were extracted by auto solid phase extraction (SPE), separated by the Allure PFP propyl column with a mobile phase consisting of methanol and 20 mmol/L ammonium acetate buffer [0.1% formic acid (80:20, V/V)], and then analyzed by LC-MS/MS. Multiple reaction monitoring (MRM) mode was used to analyze COC (m/z 304.2-->182.3, m/z 304.2-->150.1) and BZE (m/z 290.2-->168.3, m/z 290.2-->105.0).
RESULTS:
COC and BZE showed a fairly good linearity over the range of 2.0-100 ng/mL (r=0.9995). The detection limit was 0.5 ng/mL. The recovery rate was greater than 90% and the deviation of intra- and inter-day precision was less than 6%. BZE was the major target detected in urine samples, and its detection window was longer than COC.
CONCLUSION
This newly developed method shows high sensitivity and selectivity, and is suitable for the simultaneous analysis of cocaine and benzoylecgonine in urine samples.
Animals
;
Chromatography, Liquid/methods*
;
Cocaine/urine*
;
Forensic Toxicology
;
Guinea Pigs
;
Humans
;
Solid Phase Extraction
;
Tandem Mass Spectrometry/methods*
7.Simultaneous determination of clozapine, olanzapine and mirtazapine in human plasma by LC-MS/MS.
Xian-Qin WANG ; Xiao-Jun PAN ; Guan-Yang LIN ; Zheng XIANG ; Xue-Bao WANG ; Jian-Zhang WU ; Dan LIN
Journal of Forensic Medicine 2009;25(2):123-126
OBJECTIVE:
To develop a method for determination of clozapine, olanzapine and mirtazapine in human plasma by liquid chromatography-tandem mass spectrometry(LC-MS/MS).
METHODS:
Clozapine, olanzapine and mirtazapine were extracted from plasma samples by using diethyl ether and separated by Agilent Zorbax SB-C18 column(2.1 mm x 150 mm, 5 microm). Electrospray ionization source was applied, positive ion mode was used to detect and multiple reaction monitoring mode was used to quantify clozapine, olanzapine and mirtazapine. Carbamazepine was the internal standard.
RESULTS:
The detection limits of clozapine, olanzapine and mirtazapine were within 0.41-0.92 ng/mL. The calibration curve in the concentration range of 10.0-2000.0 ng/mL showed a good linear distribution (r > or = 0.992 4). The average extraction recoveries were within 65.7%-94.2%. Intra-day RSD and inter-day RSD were less than 6% (n = 5).
CONCLUSION
This method seems to be quite specific, sensitive and accurate, and can be used to detect clozapine, olanzapine and mirtazapine in forensic and clinical analytic toxicology.
Benzodiazepines/blood*
;
Chromatography, Liquid/methods*
;
Clozapine/blood*
;
Forensic Toxicology
;
Humans
;
Mianserin/blood*
;
Mirtazapine
;
Olanzapine
;
Tandem Mass Spectrometry/methods*
8.The Role of Segmental Analysis of Clonazepam in Hair in Drug Facilitated Cases.
Hang CHEN ; Ping XIANG ; Min SHEN
Journal of Forensic Medicine 2017;33(3):252-257
OBJECTIVES:
To infer the frequency of dosage and medication history investigate of the victims in drug facilitated cases by the segmental analysis of clonazepam in hair.
METHODS:
Freezing milling under liquid nitrogen environment combined with ultrasonic bath was used as sample pretreatment in this study, and liquid chromatography-tandem mass spectrometry was used for the segmental analysis of the hair samples collected from 6 victims in different cases. The concentrations of clonazepam and 7-aminoclonazepam were detected in each hair section.
RESULTS:
Clonazepam and its metabolite 7-aminoclonazepam were detected in parts of hair sections from the 6 victims. The occurrence time of drug peak concentration was consistent with the intake timing provided by victims.
CONCLUSIONS
Segmental analysis of hair can provide the information of frequency of dosage and intake timing, which shows an unique evidential value in drug facilitated crimes.
Adult
;
Chromatography, Liquid
;
Clonazepam/analysis*
;
Crime
;
Forensic Medicine/methods*
;
Forensic Toxicology
;
Hair/chemistry*
;
Humans
;
Mass Spectrometry
;
Spectrometry, Mass, Electrospray Ionization
;
Substance Abuse Detection/methods*
;
Ultrasonics
9.Analysis of paraquat in blood and urine by sodium borohydride/nickel chloride chemical reduction-gas chromatography/thermionic specific detector.
Lu-Yao HUANG ; Lin-chuan LIAO ; Li-Li CHEN ; Gui SU ; Wen-Jia LI ; Rong HE ; You-Yi YAN ; Lin YANG
Journal of Forensic Medicine 2008;24(6):429-432
OBJECTIVE:
To establish a new method for the analysis of paraquat in blood and urine by sodium borohydride/nickel chloride chemical reduction-gas chromatography/thermionic specific detector.
METHODS:
An initial procedure of precipitation was performed by adding hydrochloric solution with sodium chloride and a mixture of chloroform and ethanol. Then the analyte contained in supernatant was reduced by a reduction system of sodium borohydride and nickel chloride and extracted by acetic ether. Ethyl paraquat (EPQ) was used as internal standard. GC/TSD was used to identify and quantify the analyte.
RESULTS:
The limits of detection (S/N=3) in blood and urine were 0.002 and 0.004 microg/mL, respectively. The linear ranges were 0.050-30.0 microg/mL. Correlation coefficients in blood and urine were 0.999 and 0.998, respectively. The recoveries exceeded 80% both in blood and urine.
CONCLUSION
This method is applicable for quantification of paraquat in biological fluids.
Borohydrides/chemistry*
;
Chromatography, Gas/methods*
;
Forensic Toxicology
;
Herbicides/urine*
;
Humans
;
Nickel/chemistry*
;
Oxidation-Reduction
;
Paraquat/urine*
;
Sensitivity and Specificity
10.Determination of Cr, Cd, As, Tl and Pb in blood by inductively coupled plasma mass spectrometry.
Dong MA ; Min SHEN ; Xian-yi ZHUO ; Hui YAN ; Ping XIANG ; Wei LIU
Journal of Forensic Medicine 2009;25(1):37-39
OBJECTIVE:
To establish an inductively coupled plasma mass spectrometry (ICP-MS) method for determination of Cr, Cd, As, Tl and Pb in blood.
METHODS:
The samples were digested by microwave digestion instrument. ICP-MS was applied to determine Cr, Cd, As, Tl and Pb in blood by using 115In as an internal standard.
RESULTS:
The limits of detection were in the range of 0.00001-0.00249 microg/L. The accuracy of the method ranged from 90.1% to 110.7% and the precision ranged from 4.0% to 7.9%.
CONCLUSION
The method is accurate and rapid with superior sensitivity and linear range. It could be used in the poisoning cases caused by Cr, Cd, As, Tl and Pb.
Arsenic/blood*
;
Cadmium/blood*
;
Chromium/blood*
;
Forensic Toxicology
;
Humans
;
Lead/blood*
;
Mass Spectrometry/methods*
;
Metals, Heavy/blood*
;
Titanium/blood*