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HPLC-MS/MS法同时测定清开灵口服液中7种成分的含量
Simultaneous Determination of 7 Components in Qingkailing Oral Liquid by HPLC-MS/MS
【摘要】 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,1.7μm);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7.775~93.30μg·m L-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·m L-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。
【Abstract】 ObjectiveAn HPLC-MS/MS method was established for the simultaneous determination of 7 components in Qingkailing Oral Liquid.MethodsThe assay was performed on a Waters ACQUITY UPLC BEH C18column(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.ResultsThe 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.ConclusionThe 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.
【Key words】 QingkailingOral Liquid; adenosine; chlorogenic acid; caffeic acid; geniposide; baicalin; hyodeoxycholic acid; cholic acid; HPLC-MS/MS; content determination;
- 【文献出处】 中药新药与临床药理 ,Traditional Chinese Drug Research and Clinical Pharmacology , 编辑部邮箱 ,2024年02期
- 【分类号】R286.0
- 【下载频次】248