超高效液相色谱-串联质谱法测定毛发中7种新型苯二氮[艹卓]类策划药物的含量  

Determination of 7 Novel Designer Benzodiazepines in Hair by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：郑新勇 曹广生 王辰雪 刘宸 李旭阳 宋昕[1] ZHENG Xinyong;CAO Guangsheng;WANG Chenxue;LIU Chen;LI Xuyang;SONG Xin(Institute of Criminal Science and Technology of Hefei Public SecurityBureau,Hefei 23000l,China;Hangzhou EXPEC Technology Co.,Ltd.,Hangzhou 31oooo,China)

机构地区：[1]合肥市公安局刑事科学技术研究所,合肥230001 [2]杭州谱育科技发展有限公司,杭州310000

出　　处：《理化检验（化学分册）》2023年第12期1425-1430,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：由于新型苯二氮[艹卓]类策划药物具有用量小、药效强、体内代谢快和含量低等特点,很难在受害人的血液和尿液中检出,而毛发具有检出时效长、易获取和易保存的优势,因此提出了题示方法.取剪至1~2 mm的毛发20 mg,加入1 m L含内标(1μg.L^(-1)阿普唑仑Gd5)提取剂,于-50℃预冷5min,冷冻研磨两次,每次90s,中间间隔60s,并离心5min,取上清液浓缩至干,用100μL甲醇复溶,经0.22μm有机滤膜过滤.滤液在Acquity UPLCHSST3色谱柱上进行分离,经不同体积比的0.1%(体积分数,下同)甲酸溶液G含0.1%甲酸的乙腈溶液的混合液为流动相进行梯度洗脱,采用电喷雾离子源正离子模式(ESI+)扫描,多反应监测(MRM)模式检测,以保留时间和特征离子定性,内标法定量.结果表明,7种新型苯二氮[艹卓]类策划药物(瑞马唑仑、科纳唑仑、氟阿普唑仑、氟溴唑仑、玻玛唑仑、依替唑仑、溴替唑仑)工作曲线的线性范围为1~500pg.mg^(-1),检出限(3S/N)为0.11~0.35pg.mg^(-1).按照标准加入法进行回收试验,回收率为90.2%~104%,日内精密度和日间精密度试验所得相对峰面积的相对标准偏差(n=6)分别为1.7%~4.7%和2.9%~7.0%.Due to the characteristics of small dosage,strong efficacy,fast metabolism in the body,and low content of novel designer benzodiazepines,it was difficult to detect them in the blood and urine of victims.Hair had the advantages of long detection time,easy acquisition,and easy preservation.Therefore,the title method was proposed.20 mg of hair cut to 1-2 mm was taken,and 1 mL of extract containing internal standard(1μg·L^(-1)alprazolam-d,)was added.The mixture was pre-cooled at-50℃for 5 min,frozen and ground twice(each time for 90 s,with an interval of 60 s),and centrifuged for 5 min.The supernatant was taken and concentrated to dryness,and the residue was redissolved in 100μL of methanol.The solution was filtered by 0.22μm organic filter membrane filtration,and the filtrate was separated on the Acquity UPLC HSS T3 column,with a mixture of o.1%(volume fraction,the same below)formic acid solution and acetonitrile solution containing o.1%formic acid at different volume ratios as the mobile phase for gradient elution.The electrospray ion source positive ion(ESI+)mode was used for scanning and multiple reaction monitoring(MRM)mode was used for detection,with qualitative analysis by retention time and characteristic ions and quantitative analysis by internal standard method.As shown by the results,linear range of working curves for 7 novel designer benzodiazepines(remimazolam,clonitrazolam,flualprazolam,bromazolam,flubromazolam,etizolam,and brotizolam)was 1-500 pg·mg^(-1),with detection limits(3S/N)in the range of o.11-0.35 pg·mg^(-1).Test for recovery was made by standard addition method,giving results in the range of 90.2%-104%,with RSDs(n=6)relative peak areas in the ranges of of 1.7%-4.7%for intra-day precision test and 2.9%-7.0%for inter-day precision test,respectively.

关 键 词：新型苯二氮[艹卓]类策划药物 药物辅助犯罪 毛发 超高效液相色谱G串联质谱法 

分 类 号：O657.63[理学—分析化学]