超高效液相色谱-质谱法测定芪苈强心胶囊中12种活性成分
[Determination of twelve active compounds in Qili Qiangxin capsules by UPLC-MS].
作者信息
Liu Ying, Ouyang Yue, Li Song, Liu Min-Yan, Qiao Li, Zhao Shao-Hua
出版信息
Zhongguo Zhong Yao Za Zhi. 2014 May;39(10):1822-5.
In order to establish an UPLC-MS method for determination of twelve active compounds in Qili Qiangxin capsules including astragaloside, calycosin-7-0-glucoside, ginsenoside Rb1, ginsenoside Re, ginsenoside Rd, ginsenoside Rg1, ginsenoside Rf, periplocin, periplocoside H1, hesperidin, narirutin, isoquercitrin, the chromatographic separations were performedon a Phenomenex UPLC Kinetex C18 column (2.1 mm x 100 mm, 2.6 microm) with gradient elution of acetonitrile and 0.1% aqueous formic acidat a flow rate of 0.4 mL x min(-1). The temperature was set as 40 degrees C and injection volume was 5 microL. The monitoring of all analytes was achieved under the negative ionization mode with TOF-MS and TOF-MS/MS method. The twelve analytes showed good linearity (R2 > 0.9990) within the test ranges, the average recoveries were 98.0%-102%, respectively, and the RSD were less than 3.9%, respectively. The established method is simple, rapid, and sensitive, and can be used for quality control of Qili Qiangxin capsules.
为建立一种用于测定芪苈强心胶囊中12种活性成分（包括黄芪甲苷、毛蕊异黄酮葡萄糖苷、人参皂苷Rb1、人参皂苷Re、人参皂苷Rd、人参皂苷Rg1、人参皂苷Rf、杠柳毒苷、杠柳苷H1、橙皮苷、柚皮苷、异槲皮苷）的超高效液相色谱-质谱联用（UPLC-MS）方法，采用Phenomenex UPLC Kinetex C18柱（2.1 mm×100 mm，2.6μm），以乙腈和0.1%甲酸水溶液进行梯度洗脱，流速为0.4 mL·min⁻¹。柱温设定为40℃，进样量为5μL。采用飞行时间质谱（TOF-MS）和飞行时间串联质谱（TOF-MS/MS）方法在负离子模式下对所有分析物进行监测。12种分析物在测试范围内均呈现良好的线性关系（R²＞0.9990），平均回收率分别为98.0% - 102%，相对标准偏差（RSD）均小于3.9%。所建立的方法简便、快速、灵敏，可用于芪苈强心胶囊的质量控制。
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