Determination of 7 Novel Designer Benzodiazepines in Hair by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry
摘 要
由于新型苯二氮䓬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 mL含内标(1 μg·L-1阿普唑仑-d5)提取剂,于-50℃预冷5 min,冷冻研磨两次,每次90 s,中间间隔60 s,并离心5 min,取上清液浓缩至干,用100 μL甲醇复溶,经0.22 μm有机滤膜过滤。滤液在Acquity UPLC HSS T3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-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种新型苯二氮䓬类策划药物(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1~500 pg·mg-1,检出限(3S/N)为0.11~0.35 pg·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%。
Abstract
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 (1 μg·L-1 alprazolam-d5) 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 100 μL of methanol. The solution was filtered by 0.22 μm organic filter membrane filtration, and the filtrate was separated on the Acquity UPLC HSS T3 column, with a mixture of 0.1% (volume fraction, the same below) formic acid solution and acetonitrile solution containing 0.1% 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 0.11-0.35 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.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202312010
所属栏目 工作简报
基金项目
收稿日期 2022/12/20
修改稿日期
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联系人作者宋昕(hflhsx@163.com)
备注郑新勇,高级工程师,研究方向为毒物毒品、微量物证检验技术
引用该论文: ZHENG Xinyong,CAO Guangsheng,WANG Chenxue,LIU Chen,LI Xuyang,SONG Xin. Determination of 7 Novel Designer Benzodiazepines in Hair by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(12): 1425~1430
郑新勇,曹广生,王辰雪,刘宸,李旭阳,宋昕. 超高效液相色谱-串联质谱法测定毛发中7种新型苯二氮䓬类策划药物的含量[J]. 理化检验-化学分册, 2023, 59(12): 1425~1430
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【4】钱振华,郑晓雨,刘翠梅.苯二氮卓类新精神活性物质去氯依替唑仑的定性检验方法研究[J].中国司法鉴定, 2020(1):49-53.
【5】陈航,向平,沈敏.头发中氯硝西泮的分段分析在药物辅助犯罪案件中的作用[J].法医学杂志, 2017,33(3):252-257.
【6】UNODC. NPS threats Volume IV[R]. [S.l.]:UNODC, 2021.
【7】国家毒品问题治理研究中心.我国管制毒品目录[EB/OL]. (2021-06-26) [2022-07-15]. https://dcppc.swupl.edu.cn/jddt/305235.htm.
【8】崔小培.药物辅助犯罪案件所涉药物的头发分析及评价研究[D].苏州:苏州大学, 2013.
【9】李超,王继芬,王燕燕.毛发样本的前处理技术研究进展[J].药物分析杂志, 2020,40(3):401-412.
【10】何昕宇,王继芬,王燕燕.毛发分析前处理在法庭科学中应用进展及挑战[J].化学研究与应用, 2021,33(2):209-217.
【11】黄钰,张婷婷,胡爽,等.超高效液相色谱-串联质谱法同时检测毛发中112种合成大麻素类物质[J].质谱学报, 2022,43(4):426-437.
【12】胡骏杰,郝敬梅,刘飞,等.超高效液相色谱-串联质谱结合内标法快速检测毛发中15种毒品及代谢物[J].分析科学学报, 2021,37(3):287-294.
【13】陈顺琴,唐美,黄江,等.超声提取-超高效液相色谱-串联质谱法测定毛发中常见毒品及代谢物的含量[J].理化检验-化学分册, 2022,58(1):58-64.
【14】施晓露,乔宏伟,吴健美,等.毛发中地佐辛、杜冷丁的UPLC-MS/MS检测[J].中国药科大学学报, 2022,53(1):74-78.
【15】白利文,王爱华,于忠山,等.超高效液相色谱-串联质谱法测定血液中20种常见毒品[J].理化检验-化学分册, 2019,55(11):1266-1273.
【16】钟世欢,金建奇,叶磊海,等.固相萃取柱净化-超高效液相色谱-串联质谱法测定助眠类保健品中22种禁用安神类药物的含量[J].理化检验-化学分册, 2020,56(1):1-6.
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