超高效液相串联质谱法同时测定乳块消颗粒中6种成分的含量

陈伟康,马双成,罗跃华,吴燕红,许妍*

中国药学杂志 ›› 2015, Vol. 50 ›› Issue (7) : 629-633.

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中国药学杂志 ›› 2015, Vol. 50 ›› Issue (7) : 629-633. DOI: 10.11669/cpj.2015.07.014
论著

超高效液相串联质谱法同时测定乳块消颗粒中6种成分的含量

  • 陈伟康1,马双成2,罗跃华1,吴燕红1,许妍1*
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Simultaneous Determination of Six Constituents in Rukuaixiao Granules by UHPLC-MS/MS

  • CHEN Wei-kang1, MA Shuang-cheng2, LUO Yue-hua1, WU Yan-hong1, XU Yan1*
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摘要

目的 建立超高效液相串联质谱法测定乳块消颗粒中橘红素、橙皮素、5-去甲基川陈皮素、川陈皮素、牡荆素、芸香柚皮苷的含量测定方法。方法 采用Waters ACQUITY UPLC BEH C18柱( 2.1 mm×50 mm,1.7 μm),柱温50 ℃;以乙腈(含体积分数0.1%甲酸)-体积分数0.1%甲酸溶液为流动相,流速 0.6 mL·min-1梯度洗脱;质谱以电喷雾离子源多反应监测模式(MRM)对待测物质进行测定。结果 6个成分色谱峰面积与对照品浓度之间在线性范围内呈现良好的线性关系,r>0.995 8;定量限分别为0.80、1.10、1.30、0.66、2.00、7.10、0.70 ng·mL-1;样品加样回收率在95.78%~101.35%之间,RSD均小于2.1%。 结论 该方法简便,快速、灵敏、专属性强,可为乳块消颗粒质量控制提供依据。

Abstract

OBJECTIVE To establish a UHPLC-MS/MS method for simultaneous determination of tangertin, hesperetin, 5-demethylnobiletin, nobiletin, vitexin, and narirutin in Rukuaixiao granules.METHODS The analysis method was performed on a Waters ACQUITY UPLC BEH C18 column(2.1 mm×50 mm,1.7 μm)with gradient elution of acetonitrile(containing 0.1% formic acid)-0.1% formic acid at a flow rate of 0.6 mL·min-1, and the column temperature was set at 50 ℃. Electrospray ionization (ESI) source with positive mode and the detector with multiple reaction monitoring (MRM) mode were adopted to determine the analytes by mass spectormeter.RESULTS Satisfactory linearities were obtained for the six constituents in the investigated ranges (r>0.995 8). The lower limit of quantitation (LOQ) was 0.80, 1.10, 1.30, 0.66, 2.00, 7.10 and 0.70 ng·mL-1, respectively. All the recoveries of samples were between 95.78%-101.35% with RSDs less than 2.1%.CONCLUSION The method is simple, rapid, sensitive, and highly reproducible. It can be applied to the quality control of Rukuaixiao granules.

关键词

乳块消颗粒 / 超高效液相串联质谱法 / 橘红素 / 橙皮素 / 5-去甲基川陈皮素 / 川陈皮素 / 牡荆素 / 芸香柚皮苷

Key words

Rukuaixiao grannles / UHPLC-MS/MS / tangertin / hesperetin / 5-demethylnobiletin / nobiletin / vitexin / narirutin

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陈伟康,马双成,罗跃华,吴燕红,许妍*. 超高效液相串联质谱法同时测定乳块消颗粒中6种成分的含量[J]. 中国药学杂志, 2015, 50(7): 629-633 https://doi.org/10.11669/cpj.2015.07.014
CHEN Wei-kang, MA Shuang-cheng, LUO Yue-hua, WU Yan-hong, XU Yan*. Simultaneous Determination of Six Constituents in Rukuaixiao Granules by UHPLC-MS/MS[J]. Chinese Pharmaceutical Journal, 2015, 50(7): 629-633 https://doi.org/10.11669/cpj.2015.07.014
中图分类号: R927   

参考文献

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