HPLC-MS/MS Determination of Taxol and Cephalomannine in Liquor
摘 要
将自制的红豆杉果酒注入质谱仪,确定红豆杉在白酒中的特征成分为紫杉醇和三尖杉宁碱。红豆杉酒样品用70%(体积分数)甲醇溶液稀释,离心后,采用高效液相色谱-串联质谱法测定上清液中紫杉醇和三尖杉宁碱的含量。以ACQUITY UPLC R BEH C18色谱柱(2.1 mm×50 mm,1.7 μm)为固定相,以不同体积比的甲醇和水的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源正离子模式和多反应监测模式。紫杉醇和三尖杉宁碱的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3S/N)均为2.5 μg·kg-1,测定下限(10S/N)均为8.3 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为96.4%~116%,测定值的相对标准偏差(n=6)为1.1%~2.6%。
Abstract
The self-made Taxus fruit wine was injected into mass spectrometry, and the characteristic components of Taxus in liquor were determined as taxol and cephalomannine. The Taxus wine sample was diluted with 70% (φ) methanol solution. After centrifugation, HPLC-MS/MS was applied to the determination of taxol and cephalomannine in the supernatant. ACQUITY UPLC R BEH C18 chromatographic column (2.1 mm×50 mm, 1.7 μm) was used as stationary phase, and the mixture of methanol and water mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of taxol and cephalomannine were kept in definite ranges, with same detection limits (3S/N) of 2.5 μg·kg-1 and same lower limits of determination (10S/N) of 8.3 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 96.4%-116%, with RSDs (n=6) of determined values in the range of 1.1%-2.6%.[WT5HZ]
中图分类号 O657.63 DOI 10.11973/lhjy-hx202010004
所属栏目 试验与研究
基金项目 福建省科技计划项目(2018Y0086)
收稿日期 2020/5/14
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备注陈章捷,高级工程师,硕士,主要从事食品安全质量检验工作,chenzhangj@163.com
引用该论文: CHEN Zhangjie. HPLC-MS/MS Determination of Taxol and Cephalomannine in Liquor[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(10): 1067~1072
陈章捷. 高效液相色谱-串联质谱法测定白酒中紫杉醇和三尖杉宁碱[J]. 理化检验-化学分册, 2020, 56(10): 1067~1072
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【3】刘先芳,梁敬钰,孙建博.紫杉醇:具有里程碑意义的天然抗癌药物[J].世界科学技术(中医药现代化), 2017,19(6):941-949.
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【6】PRAKASH P, KARTHICK RAJA NAMASIVAYAM S. Anti oxidative and anti tumour activity of biomass extract of mycoprotein Fusarium venenatum[J]. African Journal of Microbiology Research, 2013,7(17):1697-1702.
【7】王芳,李玉姐.紫杉醇中毒致恶性心律失常1例护理体会[J].基层医学论坛, 2017,21(27):3644-3644.
【8】刘爱华.抗肿瘤药紫杉醇的临床应用及不良反应[J].中国伤残医学, 2013,21(8):273-274.
【9】赵丽杰,吴红杰.抗肿瘤药紫杉醇的不良反应及临床合理用药分析[J].中国医药指南, 2018,16(9):140-141.
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