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Determination of higenamine in multi-matrix by gas chromatography-mass spectrometry combined with derivatization technology
Journal of Food and Drug Analysis ( IF 2.6 ) Pub Date : 2020-01-01 , DOI: 10.1016/j.jfda.2019.09.002 Yan-Ru Feng 1 , Bo Wang 2 , Guo-Jun Li 3 , Wei-Jun Kang 1 , Kao-Qi Lian 4 , Xin-Li Lu 5
Journal of Food and Drug Analysis ( IF 2.6 ) Pub Date : 2020-01-01 , DOI: 10.1016/j.jfda.2019.09.002 Yan-Ru Feng 1 , Bo Wang 2 , Guo-Jun Li 3 , Wei-Jun Kang 1 , Kao-Qi Lian 4 , Xin-Li Lu 5
Affiliation
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Higenamine (HG), a cardioactive component of some foods and medicines, has been listed in the doping category by the International Olympic Committee, which may lead to misuse by athletes. We report the development of a gas chromatography-mass spectrometry (GC-MS) method for determination of HG in various matrix samples (biological samples, different forms of Chinese patent medicine, Chinese herbal medicine) based on acylation derivatization of HG by heptafluorobutyric anhydride. Under optimal conditions, the linearity of HG in the range of 5-200 ng mL-1 was acceptable (R2 > 0.999), and the limit of detection (LOD) and limit of quantitation (LOQ) for HG was 1.52 ng mL-1 and 5 ng mL-1, respectively. Low, medium, and high concentrations (25, 100 and 160 ng mL-1) of HG were added to plasma, urine, oral liquid, capsule, watered bolus, honeyed bolus and Chinese herbal medicine samples, with recovery ranging from 82.70 to 109.80%, intra-day and inter-day precisions were both less than 3.39%. The results indicated that the method had sufficient sensitivity for analysis of biological samples, and Chinese patent and herbal medicine.
中文翻译：
气相色谱-质谱联用衍生化技术测定多基质中的higenamine
Higenamine (HG) 是一些食品和药物的心脏活性成分，已被国际奥委会列入兴奋剂类别，这可能会导致运动员滥用。我们报告了基于七氟丁酸酐酰化衍生化 HG 的气相色谱-质谱 (GC-MS) 测定方法的开发，该方法用于测定各种基质样品（生物样品、不同形式的中成药、中草药）中的 HG。在最佳条件下，HG 在 5-200 ng mL-1 范围内的线性可接受（R2 > 0.999），HG 的检测限 (LOD) 和定量限 (LOQ) 为 1.52 ng mL-1和 5 ng mL-1，分别。将低、中和高浓度（25、100 和 160 ng mL-1）的 HG 添加到血浆、尿液、口服液、胶囊、水丸、蜜丸和中草药样品，回收率为82.70%～109.80%，日内和日间精密度均小于3.39%。结果表明，该方法对生物样品、中成药和中草药的分析具有足够的灵敏度。
更新日期：2020-01-01
中文翻译：
气相色谱-质谱联用衍生化技术测定多基质中的higenamine
Higenamine (HG) 是一些食品和药物的心脏活性成分，已被国际奥委会列入兴奋剂类别，这可能会导致运动员滥用。我们报告了基于七氟丁酸酐酰化衍生化 HG 的气相色谱-质谱 (GC-MS) 测定方法的开发，该方法用于测定各种基质样品（生物样品、不同形式的中成药、中草药）中的 HG。在最佳条件下，HG 在 5-200 ng mL-1 范围内的线性可接受（R2 > 0.999），HG 的检测限 (LOD) 和定量限 (LOQ) 为 1.52 ng mL-1和 5 ng mL-1，分别。将低、中和高浓度（25、100 和 160 ng mL-1）的 HG 添加到血浆、尿液、口服液、胶囊、水丸、蜜丸和中草药样品，回收率为82.70%～109.80%，日内和日间精密度均小于3.39%。结果表明，该方法对生物样品、中成药和中草药的分析具有足够的灵敏度。
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