HPLC-MS/MS同时测定芪龙胶囊中6个有效成分的含量

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II_A、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II_A、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II_A、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。

Objective: To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneous determination of salvianolic acid B,paeoniflorin, tanshinone II_A,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 II_A,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 II_A,astragaloside A,amygdalin and calycosin-7-glucoside in Qilong capsules. It can be used for the quality control of Qilong capsules.

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