LC-MS/MS法同时测定参芍胶囊中人参皂苷和芍药苷的含量

目的：建立高效液相色谱-串联质谱（LC-MS/MS）法同时测定参芍胶囊中人参皂苷Rb₂、Rd、Re、Rg₁和芍药苷的含量。方法：采用Hypersil Gold C₁₈色谱柱（2.1 mm×100 mm，3 μm），以乙腈-0.1%甲酸水溶液为流动相，梯度洗脱（0~10 min，15%乙腈→40%乙腈；10~13 min，40%乙腈→70%乙腈），流速0.3 mL·min^-1，柱温40℃；采用电喷雾离子源（ESI），多反应监测（MRM）模式，负离子检测。结果：人参皂苷Rb₂、Rd、Re、Rg₁和芍药苷的线性范围分别为0.01~12.66 μg·mL^-1（r=0.999 7）、0.01~10.34 μg·mL^-1（r=0.999 6）、0.02~17.44 μg·mL^-1（r=0.999 1）、0.02~17.29 μg·mL^-1（r=0.999 1）和0.01~11.76 μg·mL^-1（r=0.999 9），平均加样回收率（n=6）均在96.8%~100.1%范围内。3批样品中人参皂苷Rb₂、Rd、Re、Rg₁和芍药苷的含量测定结果分别为3.903~3.990、6.555~6.628、10.69~11.42、7.024~8.381和84.65~86.87 mg·g^-1。结论：所建立的方法可用于参芍胶囊的质量控制。

Objective:To establish an LC-MS/MS method for simultaneous determination of ginsenoside Rb₂,ginsenoside Rd,ginsenoside Re,ginsenoside Rg₁ and paeoniflorin in Shenshao capsules by LC-MS/MS. Methods:The chromatographic separation was performed on a Hypersil Gold C₁₈ column(2.1 mm×100 mm, 3 μm)with a mobile phase consisting of acetonitrile-0.1% formic acid at the flow rate of 0.3 mL·min^-1(0-10 min,15% acetonitrile→40% acetonitrile;10-13 min,40% acetonitrile→70% acetonitrile).The column temperature was 40℃.Negative electrospray ionization source(ESI)was used combined with multiple reaction monitoring(MRM).Results:Good linearity was obtained in the range of 0.01-12.66 μg·mL^-1(r=0.999 7)for ginsenoside Rb₂,0.01-10.34 μg·mL^-1(r=0.999 6)for ginsenoside Rd,0.02-17.44 μg·mL^-1(r=0.999 1)for ginsenoside Re,0.02-17.29 μg·mL^-1(r=0.999 1)for ginsenoside Rg₁ and 0.01-11.76 μg·mL^-1(r=0.999 9)for paeoniflorin, respectively.The average recoveries of five components were 96.8%-100.1%.The contents of ginsenoside Rb₂,ginsenoside Rd,ginsenoside Re,ginsenoside Rg₁ and paeoniflorin in 3 batches of samples were 3.903-3.990 mg·g^-1,6.555-6.628 mg·g^-1,10.69-11.42 mg·g^-1,7.024-8.381 mg·g^-1 and 84.65-86.87 mg·g^-1,respectively.Conclusion:The established method can be used for the quality control of Shenshao capsules.