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超高效液相色谱-串联质谱法同时测定海蛇药酒中11种化学成分

Simultaneous determination of 11 kinds of constituents in seasnake medicinal liquor by ultra performance liquid chromatographytandem mass spectrometry

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【作者】 汤丽昌; 尹群健; 邓世明; 梁国华; 陈高健;

【Author】 TANG Li-Chang;YIN Qun-Jian;DENG Shi-Ming;LIANG Guo-Hua;CHEN Gao-Jian;Beihai Food & Drug Inspection and Testing Institute;Fourth Institute of Oceanography,Ministry of Natural Resources;School of Life and Pharmaceutical Sciences, Hainan University;

【通讯作者】 邓世明;

【机构】 北海市食品药品检验所; 自然资源部第四海洋研究所; 海南大学生命科学与药学院;

【摘要】 目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定海蛇药酒中多种成分含量的分析方法。方法采用Agilent EC-C18色谱柱(4.6 mm×50 mm,1.8μm),以水(0.1%甲酸)-乙腈(0.1%甲酸)为流动相,梯度洗脱,流速0.2 mL/min,进样量为10μL,柱温为30℃;采用电喷雾离子源(electron spray ionization,ESI)进行正离子模式监测,多反应监测模式(multiple reaction monitoring,MRM)进行定量分析。结果 1-甲基海因、紫丁香苷、绿原酸、升麻素苷、芦丁、香草酸、木犀草苷、阿魏酸、黄芩苷、槲皮素、蛇床子素分别在0.1234~6.170(r=0.9991)、0.03340~1.670(r=0.9996)、0.2578~12.89 (r=0.9998)、0.3220~16.10 (r=0.9992)、0.04975~2.488(r=0.9992)、0.02592~1.296(r=0.9991)、0.1001~5.005 (r=0.9991)、0.1054~5.270 (r=0.9994)、0.000685~0.03425 (r=0.9986)、0.00542~0.2710(r=0.9996)和0.2822~14.11 mg/L(r=0.9993)线性关系良好,平均回收率在97.4%~103.5%之间,精密度为0.34%~2.02%。结论该方法快速、专属性强、灵敏度高,可用于海蛇药酒的质量控制。

【Abstract】 Objective To establish a method for simultaneous determination of 11 kinds of main active components in seasnake medicinal liquor by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods UPLC-MS/MS analysis was performed on a Agilent EC-C18(4.6 mm×50 mm, 1.8 μm) eluted with acetonitrile and ultrapure water both containing 0.1% formic acid in a gradient program. The flow rate was 0.2 mL/min, the injection volume was 10 μL at column temperature 30 ℃. The multiple-reaction monitoring(MRM) scanning mode was employed for quantification with switching electrospray ion source polarity in positive mode. Results 1-Methylhydantoin, ligustrin, chlorogenic acid, prim-O-glucosylcimifugin, rutin, vanillic acid, luteoloside, ferulic acid, baicalin, quercetin, osthole showed a good linearity in the ranges of 0.1234-6.170(r=0.9991), 0.03340-1.670(r=0.9996), 0.2578-12.89(r=0.9998), 0.3220-16.10(r=0.9992), 0.04975-2.488(r=0.9992), 0.02592-1.296(r=0.9991), 0.1001-5.005(r=0.9991), 0.1054-5.270(r=0.9994), 0.000685-0.03425(r=0.9986), 0.00542-0.2710(r=0.9996) and 0.2822-14.11 mg/L(r=0.9993). The average recoveries varied from 97.4%-103.5%. The RSD values of precision varied from 0.34%-2.02%. Conclusions The method is rapid, specific and sensitive, and can be applied in the quality control of seasnake medicinal liquor.

【基金】 国家十三五海洋经济创新发展示范城市项目(HHCF20180103)~~
  • 【文献出处】 食品安全质量检测学报 ,Journal of Food Safety & Quality , 编辑部邮箱 ,2021年13期
  • 【分类号】O657.63;TS262.91
  • 【被引频次】1
  • 【下载频次】230
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