首页|HPLC-MS/MS法同时测定清开灵口服液中7种成分的含量

HPLC-MS/MS法同时测定清开灵口服液中7种成分的含量

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目的 建立高效液相色谱-质谱联用(HPLC-MS/MS)法同时测定清开灵口服液中 7 种成分含量.方法 采用 Waters ACQUITY UPLC BEH C18 色谱柱(2.1 mm×10 mm,1.7 μm);以含 10 mmol·L-1 乙酸铵和0.1%甲酸的水溶液(A)及甲醇(B)为流动相,梯度洗脱;电喷雾离子源,正、负离子多反应监测(MRM)模式进行定量分析.结果 腺苷、绿原酸、咖啡酸、栀子苷、黄芩苷、猪去氧胆酸和胆酸质量浓度分别在 0.100 4~3.213、0.784 5~8.982、0.998~3.194、0.622 5~19.92、25.05~300.6、2.513~30.15 和 7.775~93.30 μg·mL-1 范围内与峰面积呈良好线性关系(r≥0.999 0);平均回收率(n=6)分别为 100.9%、98.74%、101.2%、100.2%、100.8%、99.97%和 98.94%,RSD分别为 1.58%、0.59%、1.78%、1.25%、0.65%、1.69%和 1.07%.15 批样品中腺苷、绿原酸、咖啡酸、栀子苷、黄芩苷、猪去氧胆酸和胆酸的含量范围分别为 0.12~0.18、0.19~0.24、0.06~0.09、0.34~0.37、4.54~4.85、0.49~0.67 和 1.82~2.19 mg·mL-1.15 批样品测定结果较为接近.结论 该方法具有良好的灵敏度、准确性和重复性,可为清开灵口服液的质量控制和后续研究提供参考及数据支持.
Simultaneous Determination of 7 Components in Qingkailing Oral Liquid by HPLC-MS/MS
Objective An HPLC-MS/MS method was established for the simultaneous determination of 7 components in Qingkailing Oral Liquid.Methods The assay was performed on a Waters ACQUITY UPLC BEH C18 column(2.1 mm×10 mm,1.7 μm)and the sample was eluted with a gradient mobile phase containing 10 mmol·L-1 of ammonium acetate and 0.1%of formic acid in water(A)-methanol(B).The mass spectrometry was carried out by electrospray ionization(ESI)with positive/negative ions in multiple reaction monitoring(MRM)mode for quantitative analysis.Results The linear ranges of adenine,chlorogenic acid,caffeic acid,geniposide,baicalin,hyodeoxycholic acid and cholic acid were 0.100 4-3.213,0.784 5-8.982,0.998-3.194,0.622 5-19.92,25.05-300.6,2.513-30.15 and 7.775-93.30 μg·mL-1(r≥0.999 0).The average recoveries(n=6)were 100.9%,98.74%,101.2%,100.2%,100.8%,99.97%and 98.94%with RSD of 1.58%,0.59%,1.78%,1.25%,0.65%,1.69%and 1.07%.The contents of the above mentioned 7 components in 15 tested samples were in the ranges of 0.12-0.18,0.19-0.24,0.06-0.09,0.34-0.37,4.54-4.85,0.49-0.67 and 1.82-2.19 mg·mL-1.The contents of 7 components in tested sample from different manufacturers were closed.Conclusion The method has shown good sensitivity,accuracy,and repeatability.The study can provide reference and data support for the quality control and subsequent research of Qingkailing Oral Liquid.

Qingkailing Oral Liquidadenosinechlorogenic acidcaffeic acidgeniposidebaicalinhyodeoxycholic acidcholic acidHPLC-MS/MScontent determination

吴锦云、蔡凯伟、陈红英、王家祺、潘碧妍、谢智勇、廖琼峰

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广州中医药大学中药学院,广东广州 510006

广州白云山明兴制药有限公司,广东 广州 510250

中山大学药学院(深圳),广东 深圳 528406

清开灵口服液 腺苷 绿原酸 咖啡酸 栀子苷 黄芩苷 猪去氧胆酸 胆酸 高效液相色谱-质谱联用法 含量测定

广州市科技计划项目广州市南沙区科技计划项目

2023B03J13822022ZD004

2024

中药新药与临床药理
广州中医药大学

中药新药与临床药理

CSTPCD北大核心
影响因子:0.908
ISSN:1003-9783
年,卷(期):2024.35(2)
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