目的利用气相色谱-四极杆飞行时间质谱法(gas chromatography-quadrupole time of flight mass spectrometry,GC-QTOF-MS)鉴定药物辅助性犯罪案件样品中替来他明和唑拉西泮及其代谢物组分。方法取受害人尿样,经液液萃取后浓缩供GC-QTOF...目的利用气相色谱-四极杆飞行时间质谱法(gas chromatography-quadrupole time of flight mass spectrometry,GC-QTOF-MS)鉴定药物辅助性犯罪案件样品中替来他明和唑拉西泮及其代谢物组分。方法取受害人尿样,经液液萃取后浓缩供GC-QTOF-MS检测。通过精确质量数的测定确认碎片离子的分子式,以鉴定相关物质。结果实际案件尿样中检出替来他明、唑拉西泮、3种替来他明代谢物和2种唑拉西泮代谢物。结论 GC-QTOF-MS提供丰富准确的碎片离子质量数信息,可用于药物辅助性犯罪案件中替来他明和唑拉西泮及其代谢物的定性鉴定。展开更多
In recent years,a significant number of investigations have discovered up to 200000 unsubmitted sexual assault kits(SAKs)in the US.While the public outcry was largely directed towards DNA analysis,the SAKs also contai...In recent years,a significant number of investigations have discovered up to 200000 unsubmitted sexual assault kits(SAKs)in the US.While the public outcry was largely directed towards DNA analysis,the SAKs also contained biological specimens specifically designated for toxicological analysis.Due to the sensitivity of analytes in potential drug facilitated sexual assaults,the preservation and maintenance of the specimens is crucial in providing accurate toxicological measurements.The investigations into the unsubmitted SAKs have identified subjective law enforcement officer(LEO)rationale for the unsubmitted kits,however the impact on toxicological specimens has not been examined.This brief review of policies and guidelines with respect to forensic specimens has identified potential sources of evidentiary degradation,despite the use of chemical preservatives.With respect to temperature-controlled environments,the variation in SAK submission policies established throughout the US are potentially detrimental to the preservation of toxicological evidence.Degradation as a result of time-delayed collection and poorly maintained storage temperatures plays a crucial role for/in the interpretation of qualitative and quantitative toxicological results.This review finds these delays can be addressed through modernisation of facilities;electronic tracking of unsubmitted SAKs;mandated transfer of biological evidence within 72 h;and documentation of temperature within the chain of custody or other records.Without identifying the range of temperatures in which the evidence was exposed,forensic toxicologists may unintentionally provide erroneous interpretations of toxicological analyses-potentially casting doubt on the survivor’s recall of events and negatively impacting future sexual assault investigations.展开更多
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^(...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%.展开更多
文摘目的利用气相色谱-四极杆飞行时间质谱法(gas chromatography-quadrupole time of flight mass spectrometry,GC-QTOF-MS)鉴定药物辅助性犯罪案件样品中替来他明和唑拉西泮及其代谢物组分。方法取受害人尿样,经液液萃取后浓缩供GC-QTOF-MS检测。通过精确质量数的测定确认碎片离子的分子式,以鉴定相关物质。结果实际案件尿样中检出替来他明、唑拉西泮、3种替来他明代谢物和2种唑拉西泮代谢物。结论 GC-QTOF-MS提供丰富准确的碎片离子质量数信息,可用于药物辅助性犯罪案件中替来他明和唑拉西泮及其代谢物的定性鉴定。
文摘In recent years,a significant number of investigations have discovered up to 200000 unsubmitted sexual assault kits(SAKs)in the US.While the public outcry was largely directed towards DNA analysis,the SAKs also contained biological specimens specifically designated for toxicological analysis.Due to the sensitivity of analytes in potential drug facilitated sexual assaults,the preservation and maintenance of the specimens is crucial in providing accurate toxicological measurements.The investigations into the unsubmitted SAKs have identified subjective law enforcement officer(LEO)rationale for the unsubmitted kits,however the impact on toxicological specimens has not been examined.This brief review of policies and guidelines with respect to forensic specimens has identified potential sources of evidentiary degradation,despite the use of chemical preservatives.With respect to temperature-controlled environments,the variation in SAK submission policies established throughout the US are potentially detrimental to the preservation of toxicological evidence.Degradation as a result of time-delayed collection and poorly maintained storage temperatures plays a crucial role for/in the interpretation of qualitative and quantitative toxicological results.This review finds these delays can be addressed through modernisation of facilities;electronic tracking of unsubmitted SAKs;mandated transfer of biological evidence within 72 h;and documentation of temperature within the chain of custody or other records.Without identifying the range of temperatures in which the evidence was exposed,forensic toxicologists may unintentionally provide erroneous interpretations of toxicological analyses-potentially casting doubt on the survivor’s recall of events and negatively impacting future sexual assault investigations.
