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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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HPLC-MS/MS同时测定芪龙胶囊中6个有效成分的含量

Simultaneous determination of six active ingredients in Qilong capsules by HPLC-MS/MS

分类号:R917
出版年·卷·期(页码):2020,40 (5):795-801
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立高效液相色谱-串联杆质谱法(HPLC-MS/MS)同时测定芪龙胶囊中丹参酚酸B、芍药苷、丹参酮IIA、黄芪甲苷、苦杏仁苷、毛蕊异黄酮苷6个有效成分的含量。方法:采用CAPCELL PAK C18色谱柱(2.0 mm×150 mm,5 μm),以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,流速0.4 mL·min-1,柱温30℃,进样量10 μL;质谱采用电喷雾电离源(ESI+),多反应监测模式(MRM),离子源电压5 kV,离子源温度450℃,气帘气103.4 kPa,雾化气344.7 kPa,辅助气379.2 kPa。结果:所测6个有效成分在测定质量浓度范围内线性关系良好(r>0.992 9);平均加样回收率为91.2%~104.8%,RSD为1.3%~5.1%。13批芪龙胶囊中丹参酚酸B、芍药苷、丹参酮IIA、黄芪甲苷、苦杏仁苷、毛蕊异黄酮苷的含量范围分别为0.164~0.323、0.561~0.952、0.009~0.030、0.113~0.397、0.014~0.284、0.041~0.138 mg·粒-1结论:该方法适用于芪龙胶囊成药中丹参酚酸B、芍药苷、丹参酮IIA、黄芪甲苷、苦杏仁苷、毛蕊异黄酮苷6个有效成分含量的同时测定,可用于芪龙胶囊的质量控制。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneous determination of salvianolic acid B,paeoniflorin, tanshinone IIA,astragaloside A,amygdalin and calycosin-7-glucoside in Qilong capsules. Methods: The contents of six active ingredients in Qilong capsules were determined by CAPCELL PAK C18 column (2.0 mm×150 mm, 5 μm) with 0.1% formic acid solution-acetonitrile as mobile phase using gradient elution at a flow rate of 0.4 mL·min-1. The column temperature was 30℃ and the injection volume was 10 μL. ESI+ scan combined with multi-reaction monitoring mode (MRM) was adopted and the instrument parameters were as follows:ionsource voltage:5 kV;temperature:450℃; curtain gas:103.4 kPa;atomized gas:344.7 kPa;auxiliary gas:379.2 kPa. Results: The linear relationship of the six active ingredients was good (r>0.992 9). The average recoveries were 91.2%-104.8% with RSD of 1.3%-5.1%. The contents of salvianolic acid B,paeoniflorin,tanshinone IIA,astragaloside A,amygdalin and calycosin-7-glucoside in 13 batches of Qilong capsules were 0.164-0.323,0.561-0.952,0.009-0.030,0.113-0.397,0.014-0.284 and 0.041-0.138 mg per capsule,respectively. Conclusion: The method is suitable for the simultaneous determination of salvianolic acid B,paeoniflorin,tanshinone IIA,astragaloside A,amygdalin and calycosin-7-glucoside in Qilong capsules. It can be used for the quality control of Qilong capsules.

-----参考文献:---------------------------------------------------------------------------------------
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