LC-MS/MS法同时测定参芍胶囊中人参皂苷和芍药苷的含量  被引量:9

Simultaneous determination of ginsenosides and paeoniflorin in Shenshao capsules by LC-MS/MS

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作  者:孙大赢 赵文法 李广华 潘广洲 张金龙 

机构地区:[1]聊城市食品药品检验检测中心,聊城252000

出  处:《药物分析杂志》2018年第1期186-190,共5页Chinese Journal of Pharmaceutical Analysis

摘  要: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,3μm),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0.01~12.66μg·mL^(-1)(r=0.999 7)、0.01~10.34μg·mL^(-1)(r=0.999 6)、0.02~17.44μg·mL^(-1)(r=0.999 1)、0.02~17.29μg·mL^(-1)(r=0.999 1)和0.01~11.76μg·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Rb_2、Rd、Re、Rg_1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 RMb2,ginsenoside Rd,ginsenoside Re,ginsenoside Rg1 and paeoniflorin in Shenshao capsules by LC-MS/MS.ethods :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 ℃.NeRgative electrospray ionization source(ESI)was used combined with multiple reaction monitoring(MRM).esults: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,ginsen-oside Rd,ginsenoside Re,1 ginsenoside Rg1 and paeoniflorin in 3 batches of samples were 3.903-3.990 mg·g1,6.555-6.628 mg·g-,10.69-11.42 mg·g^-1,Cion7.024-8.381 mg·g^-1 and 84.65-86.87 mg·g^-1,respectively.onclus:The established method can be used for the quality control of Shenshao capsules.

关 键 词:参芍胶囊 人参茎叶总皂苷 白芍 人参皂苷Rb2 人参皂苷RD 人参皂苷RE 人参皂苷Rg1 芍药苷 中药多组分含量测定 液相色谱-质谱联用 

分 类 号:R917[医药卫生—药物分析学]

 

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