首页|气相色谱-三重四极杆质谱测定全血中5种常见兽用麻醉剂

气相色谱-三重四极杆质谱测定全血中5种常见兽用麻醉剂

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本文采用程序升温进样技术结合气相色谱-三重四极杆质谱仪建立了全血中的5种常见兽用麻醉剂(替来他明、赛拉唑、氯胺酮、甲苯噻嗪、唑拉西泮)检验方法.以NaCl作为盐析剂、乙腈作为萃取剂,采用盐析辅助液液萃取法作为前处理方法,并使用小型QuEChERS净化柱对提取液进行净化.提取液采用程序升温进样技术结合气相色谱-三重四极杆质谱仪进行分析,能最大程度去除提取液体系中的乙腈溶剂.采用多反应监测模式进行检测,三组特征离子对进行定性检验,外标法进行定量分析,并对方法进行了确证.结果表明,全血中5种常见兽用麻醉剂检出限为10~20 ng/mL,定量限为20~40 ng/mL.在20~2 000 ng/mL(甲苯噻嗪为40~2 000ng/mL)范围内表现良好(r>0.998),不同浓度的添加样品回收率为71.61%~119.10%,日内精密度(RSD)为0.34%~14.81%,日间精密度(RSD)为4.03%~14.87%.本文建立的方法前处理简便、稳定性好、灵敏度高,具有广阔的开发前景,可用于实际案件检验.
Determination of Five Common Veterinary Anesthetics in Whole Blood by Gas Chromatography-triple Quadrupole Mass Spectrometry
An analytical method was established for determination of 5 common veterinary anesthetics(tiletamine,xylazole,ketamine,xylazine and zolazepam)in whole blood by using programmed temperature vaporizer(PTV)system combined GC-MS/MS.Those samples were dealt with salting-out-assisted liquid-liquid extraction(SALLE),introducing NaCl as salting-out regent and acetonitrile as extraction solvent.After that,the extracting solution was purified by QuEChERS nano column.Most acetonitrile in the solution were removed by PTV system before analyzing in GC-MS/MS for protection of gas chromatographic column.The multiple-reaction-monitoring(MRM)positive ion mode was selected for detection.Three pairs of characteristic ions were taken for qualitative analysis and external standard method was accepted for quantitative analysis.The method was verified well.The results showed that the LODs were 10-20 ng/mL and LOQs were 20-40 ng/mL.There were good linear relationships for all the analytes with correlation coefficients(r)not less than 0.998.At three spiked levels of 40,400,and 2 000 ng/mL,the recoveries for 5 veterinary anesthetics in whole blood ranged from 71.61%to 119.10%.The intra-day precision and inter-day precision of the method evaluated at the concentration of three levels ranged from 0.34%to 14.81%,4.03%to 14.87%,respectively.The developed method with broad research potential benefited its simple pretreatment,fine stability and highly sensitivity,which was applied in an actual case.

veterinary anestheticsGC-MS/MSPTVSALLEQuEChERS

董林沛、任昕昕、李佳宜、董梅

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公安部鉴定中心,北京 100038

岛津企业管理(中国)有限公司,北京 100020

兽用麻醉剂 气相色谱-三重四极杆质谱 程序升温进样 盐析辅助液液萃取 QuEChERS技术

中央级公益性科研院所基本科研业务费专项

2022JB003

2024

刑事技术
公安部物证鉴定中心

刑事技术

CSTPCD
影响因子:0.315
ISSN:1008-3650
年,卷(期):2024.49(2)
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