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超分子溶剂(SUPRASs)萃取法用于气相色谱串联质谱法检测人尿和血中的苯二氮䓬类和唑吡坦。

Supramolecular solvent (SUPRASs) extraction method for detecting benzodiazepines and zolpidem in human urine and blood using gas chromatography tandem mass spectrometry.

机构信息

Department of Legal Medicine, College of Basic Medical Sciences, Inner Mongolia Medical University, Hohhot, China.

Department of Legal Medicine, College of Basic Medical Sciences, Inner Mongolia Medical University, Hohhot, China.

出版信息

Leg Med (Tokyo). 2021 Feb;48:101822. doi: 10.1016/j.legalmed.2020.101822. Epub 2020 Nov 28.

Abstract

OBJECTIVE

A high-throughput and sensitive method using supramolecular solvent (SUPRASs) for detecting 9 benzodiazepines and zolpidem in human urine and blood by gas chromatography-tandem mass spectrometry (GC-MS/MS) was newly established and applied to authentic human urine and blood samples in this study.

METHODS

Urine and blood samples were subjected to liquid-liquid extractions with supramolecular solvent mixture which consists of tetrahydrofuran and 1-hexanol. The solvent layer was evaporated to dryness by stream of nitrogen. The residue was reconstituted with methanol, and subjected to analysis by GC-MS/MS in multiple reaction monitoring (MRM) mode; internal standard method was employed for quantifying of each targeted compound.

RESULTS

The regression equation has a good linear relationship with correlation coefficients for all tested compounds were not lower than 0.9991. The lower limits of the quantification ranged from 0.20 to 5 ng/mL for tested compounds in urine; Meanwhile, the lower limits of the quantification in this method ranged from 1 to 50 ng/mL for tested compounds in blood. These results showed that excellent reproducibility and satisfactory extraction recovery rates could be obtained for the established analytical method for 10 drugs in both blood and urine samples.

CONCLUSION

The established method in this study was high-throughput, simple and sufficiently sensitive for determining of benzodiazepinesand zolpidem in human urine and blood. Therefore, this newly established method could be of use for qualitative and quantitative determination of such drugs in urine and blood samples either for clinical poisoning monitoring or for forensic identification.

摘要

目的

本研究建立了一种使用超分子溶剂(SUPRASs)通过气相色谱-串联质谱(GC-MS/MS)检测人尿和血中 9 种苯二氮䓬类药物和唑吡坦的高通量、高灵敏度方法,并应用于真实的人尿和血样。

方法

尿样和血样用包含四氢呋喃和 1-己醇的超分子溶剂混合物进行液液萃取。溶剂层用氮气流蒸发至干。残渣用甲醇重新溶解,采用多反应监测(MRM)模式进行 GC-MS/MS 分析;采用内标法对各目标化合物进行定量。

结果

回归方程具有良好的线性关系,所有测试化合物的相关系数均不低于 0.9991。在尿中,测试化合物的定量下限范围为 0.20 至 5ng/mL;同时,在血中,测试化合物的定量下限范围为 1 至 50ng/mL。这些结果表明,该分析方法在血和尿样中对 10 种药物具有良好的重现性和令人满意的提取回收率。

结论

本研究建立的方法具有高通量、简单和足够灵敏的特点,可用于测定人尿和血中的苯二氮䓬类药物和唑吡坦。因此,该新建立的方法可用于临床中毒监测或法医鉴定中尿和血样中此类药物的定性和定量测定。

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