Quantitative analysis of thiamylal and its metabolite secobarbital using liquid chromatography?tandem mass spectrometry in adipose tissue, serum, and liver
Quantitative analysis of thiamylal and its metabolite secobarbital using liquid chromatography?tandem mass spectrometry in adipose tissue, serum, and liver
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使用液相色谱-串联质谱法定量分析脂肪组织、血清和肝脏中的硫淀粉醛及其代谢物司可巴比妥
DOI：
10.1111/1556-4029.14965
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发表时间：
2022
影响因子：
1.6
通讯作者：
Ueno Yasuhiro
中科院分区：
文献类型：
--
作者：
Yoshioka Naoki;Asano Migiwa;Kuse Azumi;Kondo Takeshi;Takahashi Motonori;Morichika Mai;Nakagawa Kanako;Sakurada Makoto;Ueno Yasuhiro
硫戊醛是一种超短效巴比妥酸盐，用于静脉给药或全身麻醉诱导。然而，已经报告了一些使用甲硫咪唑的中毒和自杀病例。此外，关于其在器官和脂肪组织中的分析的报道很少，这需要通过柱层析和蒸发进行纯化。采用液相色谱-串联质谱法（LC-MS/MS）建立了一种快速、灵敏的定量脂肪组织、血清和肝脏中硫戊醛及其代谢产物司可巴比妥的方法。使用改进的QuEChERS提取制备样品。对于脂肪组织样本，在提取中增加乙腈-己烷分配步骤。该方法被应用于调查一个可疑的自我中毒尸检病例。添加到猪心包脂肪（0.18 µg/g）、人血清（0.015 µg/mL）和猪肝（0.18 µg/g）中的硫代戊巴比妥的定量准确度分别为103%、113%和95.3%。信噪比为10时，计算的猪心包脂肪、人血清和猪肝的定量限分别为0.06 µg/g、0.005 µg/mL和0.06 µg/g。此外，在法医尸检病例中，心肌脂肪中的硫戊醛和司可巴比妥水平分别为140和1.5微克/克;血清中分别为3.5-4.9和0.12-0.20微克/毫升;肝组织中分别为6.2-42和0.58-1.1微克/克。硫戊醛尤其分布在脂肪组织中。硫代戊醛与脂肪的比例可能有助于估计从给药到死亡的时间。所开发的改进的QuEChERS提取方法与乙腈-己烷分配是适合于分析疏水性化合物，如硫代戊醛，在脂肪组织。
Thiamylal is an ultrashort‐acting barbiturate used for intravenous administration or general anesthesia induction. However, some cases of poisoning and suicide with thiamylal administration have been reported. Additionally, there are few reports on its analysis in the organs and adipose tissue, which requires purification by column chromatography and evaporation. A rapid and sensitive method was developed for quantifying thiamylal and its metabolite, secobarbital, in the adipose tissue, serum, and liver using liquid chromatography–tandem mass spectrometry (LC–MS/MS). Samples were prepared using modified QuEChERS extraction. For adipose tissue samples, an acetonitrile–hexane partitioning step was added to the extraction. This method was applied to investigate a suspected self‐poisoning autopsy case. The quantitation accuracy for thiamylal added to porcine pericardial fat (0.18 µg/g), human serum (0.015 µg/mL), and porcine liver (0.18 µg/g) was 103%, 113%, and 95.3%, respectively. The quantitation limits calculated for porcine pericardial fat, human serum, and porcine liver at a signal‐to‐noise ratio of 10 were 0.06 µg/g, 0.005 µg/mL, and 0.06 µg/g, respectively. In addition, the thiamylal and secobarbital levels in the forensic autopsy case were 140 and 1.5 µg/g, respectively, in myocardial fat; 3.5–4.9 and 0.12–0.20 µg/mL, respectively, in serum; and 6.2–42 and 0.58–1.1 µg/g, respectively, in liver tissue. Thiamylal is especially distributed in the adipose tissue. The thiamylal‐to‐fat ratio may help estimate the time from administration to death. The developed modified QuEChERS extraction method with acetonitrile–hexane partitioning is suitable for analyzing hydrophobic compounds, such as thiamylal, in the adipose tissue.