Determination of Azide Ions in Blood by Pentafluorobenzyl Derivation Followed by GC-MS / 法医学杂志

Objective To establish a method for determination of the azide ions in blood by gas chromatography-mass spectrometry （GC-MS） following pentafluorobenzyl derivatization. Methods A blood sample of 0.2 mL was placed into a 10 mL glass test tube, and the internal standard sodium cyanide, derivatization reagent pentafluorobenzyl bromide and catalyst tetradecyl benzyl dimethyl ammonium chloride were added in turn. After vortex mixing, the mixture was heated with low-power microwave for 3 min. After centrifugation, the organic phase was taken for GC-MS analysis. Results The azide ions in blood had a good linear relationship in the mass concentration range of 0.5 to 20 μg/mL. The lowest detection limit was 0.25 μg/mL and the relative recovery was 91.36%-94.58%. The method was successfully applied to a case of death from sodium azide poisoning. The mass concentration of azide ions in the blood of the dead was 11.11 μg/mL. Conclusion The method developed in this paper has strong specificity and is easy to operate, which is suitable for the rapid detection of azide ions in blood.

Identification of Tiletamine, Zolazepam and Their Metabolites in Drug Facilitated Sexual Assault by GC-QTOF-MS / 法医学杂志

Objective To identify tiletamine, zolazepam and their metabolites in samples from drug facilitated sexual assault by gas chromatography-quadrupole time of flight mass spectrometry （GC-QTOF-MS）. Methods Urine samples of victims were collected, and detected by GC-QTOF-MS after liquid-liquid extraction and concentration. The molecular formula of fragments ions was identified by determination of accurate mass numbers, to detect related substances. Results Tiletamine, zolazepam, three metabolites of tiletamine and two metabolites of zolazepam were identified in urine samples from actual cases. Conclusion GC-QTOF-MS provides abundant and accurate information of fragment ions mass numbers, which can be used for qualitative identification of tiletamine, zolazepam and their metabolites in drug facilitated sexual assault.

Simultaneous determination of trihexyphenidyl, chlorpromazine and clozapine in blood by GC-MS / 法医学杂志

OBJECTIVE@#To develop a method to measure trihexyphenidyl, chlorpromazine and clozapine in human blood with GC-MS.@*METHODS@#The specimens were alkalized (pH > 10) and extracted with V (benzene):V(ethyl acetate) = 1:1, and qualitatively analyzed using GC-MS-Full Scan with internal standard SKF525A. The specimens were alkalized (pH > 10) and extracted with V(benzene):V(ethyl acetate) = 1:1, and quantitatively analyzed using GC-MS-SIM with internal standard diazepam-d5.@*RESULTS@#The lowest detection limits of trihexyphenidyl, chlorpromazine and clozapine were 0.3, 0.3 and 0.7 ng/mL (S/N > or = 3) respectively. The calibration curve in 20-10 000 ng/mL showed a good linear distribution. The recovery rate was 79.9% to 85.5%. The RSDs of intraday and interday were less than 5.1%.@*CONCLUSION@#The established method was simple, sensitive and accurate for simultaneous determination of trihexyphenidyl, chlorpromazine and clozapine in human blood, and can be applied in forensic toxicological cases.

Coumarins from root of Zanthoxylum dimorphophyllum var. spinifolium / 中国中药杂志

<p><b>OBJECTIVE</b>To study the chemical components from dried roots of Zanthoxylum dimorphophyllum var. spinifoliun.</p><p><b>METHOD</b>The chemical components were isolated by low pressure column chromatography and their structures were identified by spectroscopic methods.</p><p><b>RESULT</b>Five compounds were isolated and identified as 6-(2', 3'-dihydroxy-3'-methyl-butyl)-7-hydroxy-5-methoxy-2H-1-benzopyran-2-one (I), 6-(2',3'-dihydroxy-3'-methyl-butyl)-7-methoxy-8-(3'-methyl-but-2'-enyl)-2H-1-benzopyran-2-one (II),6-(2',3'-dihydroxy-3'-methyl-butyl)-7-hydroxy-2H-1-benzopyran-2-one (III), 6-(2', 3'-oxiranyl-3'-methyl-butyl)-7-methoxy-8- (3-methyl-but-2-enyl)-2H-1-benzopyran-2-one (IV), 7-methoxy-8-(3'-methyl-but-2'-enyl)-2H-1-benzopyran-2-one (V).</p><p><b>CONCLUSION</b>These compounds were isolated from the plant for the first time.</p>

Studies on the coumarins in the root of Zanthoxylum dimorphophyllum / 中国中药杂志

<p><b>OBJECTIVE</b>To study the chemical constituents of the dried roots of Zanthoxylum dimorphophyllumr. spinifolium and to find out the active constituents of the plant.</p><p><b>METHOD</b>Modern chromatography was used to purify chemical constituents, and their structures were identified by various spectral methods.</p><p><b>RESULT</b>Four compounds were isolated and identified as isopimpinellin (I), xanthoxyletin (II), 6-(2', 3'-dihydroxy-3'-methyl-butyl)-7-hydroxy-2H-1-benzopyran-2-one (III), 6-(2'-O-beta-D-glucopyranosyloxy, 3'-dihydroxy-3'-methybutyl)-7-hydroxy-2H-1-benzopyran-2-one (IV).</p><p><b>CONCLUSION</b>All of the above compounds were isolated from the above mentioned plant for the first time.</p>