| LC-MS/MS法检测血液和尿液中东莨菪碱和阿托品 |
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| 作者姓名： | 刘悦鑫 田方东 李昕怡 熊根 江祥宇 李贤 李燕妮 |
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| 作者单位： | 1.昆明医科大学法医学院，云南 昆明 650500 |
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| 基金项目： | 国家重点研发计划基金资助项目（2018YFC0807201-4）；云南省创新团队科研基金资助项目（202005AE160004） |
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| 摘 要： | 目的 建立曼陀罗中毒人体血液和尿液中东莨菪碱和阿托品的LC-MS/MS检测方法。 方法 采用Shim-pack GISR-HP C18色谱柱，以乙腈-甲酸（0.1%）水溶液为流动相进行梯度洗脱，电喷雾离子源正离子多反应监测模式质谱分析，采用2个特征离子对和外标标准曲线法对曼陀罗中毒人体血液和尿液中东莨菪碱和阿托品进行定性定量分析。 结果 东莨菪碱和阿托品的定量离子对分别为m/z 304.25 M+H]+→138.15和m/z 290.2 M+H]+→124.15。东莨菪碱和阿托品在质量浓度1～100 ng/mL范围内线性良好（R≥0.999），检出限（LOD）分别为:血液0.45 ng/mL和0.19 ng/mL，尿液0.38 ng/mL和0.16 ng/mL；定量限（LOQ）分别为:血液1.01 ng/mL和0.63 ng/mL，尿液1.07 ng/mL和0.38 ng/mL；提取回收率分别为:血液94.38%和94.49%，尿液94.96%和96.52%；基质效应为-3.51%～0.84%。2种目标物的准确度为89.38%～102.86%，日内和日间精密度均小于6%。 结论 建立的LC-MS/MS检测方法能快速、准确的测定生物检材中东莨菪碱和阿托品的含量。
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| 关 键 词： | LC–MS/MS 血液 尿液 东莨菪碱 阿托品 |
| 收稿时间： | 2022-05-30 |
Determination of Scopolamine and Atropine in Blood and Urine by LC-MS / MS |
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| Affiliation: | 1.School of Forensic Medicine，Kunming Medical University，Kunming Yunnan 6505002.Yunnan Yingding Judicial Appraisal Center，Pu’er Yunnan 665000，China |
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| Abstract: | Objective To develop a LC-MS/MS method for the determination of scopolamine and atropine in human blood and urine after Datura stramonium poisoning. Methods Shim-pack GISR-HP C18 column was used for gradient elution with acetonitrile formic acid （0.1%） as the mobile phase. The electrospray ionization ion source multiple reaction monitoring mode mass spectrometry was used to analyze the scopolamine and atropine by two characteristic ion pairs and the external standard curve method. Results The quantitative ion pairs of scopolamine and atropine were m/z 304.25 M+H]+→138.15 and m/z 290.2 M+H]+→124.15, respectively. The linear range of scopolamine and atropine were 1～100 ng/mL （R≥0.999）. The limits of detection （LOD） were 0.45 ng/ml and 0.19 ng/ml in blood, 0.38 ng/ml and 0.16 ng/ml in urine; The limits of quantitation （LOQ） were 1.01 ng/ml and 0.63 ng/ml in blood, 1.07 ng/ml and 0.38 ng/ml in urine; The extraction recoveries were 94.38% and 94.49% in blood, 94.96% and 96.52% in urine; The average recoveries of the substances were 94.38% and 94.49% in matrixs. The matrix effects effect was -3.51%～0.84%. The accuracy of substances were 89.38%～102.86%, and the intra day and inter day precisions were less than 6%. Conclusions The method can be used to determine the concentration of scopolamine and atropine in biological samples quickly and accurately. |
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