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建立和验证 LC-MS/MS 法测定人血中林可霉素:在法医毒理学过敏案例中的应用。

Establishment and validation of the LC-MS/MS method for the determination of lincomycin in human blood: Application to an allergy case in forensic science.

机构信息

Jining Medical University, Jining, Shandong, China; Center of Forensic Science, Jining Medical University, Jining, 272067, Shandong, China.

Weishan People's Hospital, Jining, Shandong, China.

出版信息

J Forensic Leg Med. 2021 Jan;77:102094. doi: 10.1016/j.jflm.2020.102094. Epub 2020 Dec 6.

Abstract

An analytical method to quantify lincomycin in human blood samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed and validated. The selected method was based on a protein precipitation extraction (PPE) with methanol. Instrumental determination was carried out by LC-MS/MS, with quantification based on the internal standard method. Linearity for lincomycin was established in the concentration range of 5-100 ng/mL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.2 and 1 ng/mL, respectively. Analyte recoveries were in the range of 72.70%-84.13% for spiked blood samples. The accuracies ranged between 92.82% and 100.40%, and the intraday and inter-day precisions ranged between 1.19% and 6.40%, respectively. The developed method was applied to an authentic allergy case of lincomycin. By testing the lincomycin content in the venous blood of the deceased and combined with the pathological test results, lincomycin acute allergy appeared to be the most likely cause of death. The acquired results confirm that the developed method is capable of identifying and quantifying lincomycin in human blood and can be suitable for the detection of allergy cases in clinical or forensic science.

摘要

已开发和验证了一种通过液相色谱-串联质谱法(LC-MS/MS)定量人血样中林可霉素的分析方法。所选择的方法基于甲醇的蛋白质沉淀提取(PPE)。仪器测定通过 LC-MS/MS 进行,基于内标法进行定量。林可霉素的线性范围为 5-100ng/mL。检测限(LOD)和定量限(LOQ)分别为 0.2 和 1ng/mL。在加标血样中,分析物的回收率在 72.70%-84.13%范围内。准确度在 92.82%至 100.40%之间,日内和日间精密度分别在 1.19%至 6.40%之间。所开发的方法应用于林可霉素过敏的真实案例。通过测试死者静脉血中的林可霉素含量,并结合病理检查结果,林可霉素急性过敏似乎是最有可能的死亡原因。获得的结果证实,所开发的方法能够识别和定量人血中的林可霉素,可适用于临床或法医学过敏案例的检测。

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