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    超高效液相色谱-串联质谱法测定根痛平胶囊及片剂中松香酸和11-羰基-β-乙酰乳香酸的含量

    UHPLC-MS/MS Determination of Abietic Acid and 11-Carbonyl-β- acetyl-boswellic Acid in Gentongping Capsules and Tablets

    • 摘要: 样品0.200 0 g在乙醇中超声提取30 min,再用乙醇稀释至10.0 mL。提取液以Zorbax SB-C18色谱柱为固定相,以乙腈-0.1%(体积分数)甲酸溶液(17+3)混合液为流动相进行色谱分离。质谱分析中采用电喷雾正离子源,多反应监测模式,基质匹配制作标准曲线,外标法定量。结果表明:松香酸和11-羰基-β-乙酰乳香酸的质量浓度均在10.0~1 000 μg·L-1范围内呈线性,检出限(3S/N)分别为0.9,3.1 μg·kg-1。按标准加入法在3个浓度水平上进行加标回收试验,测得回收率在95.2%~101%之间,日内、日间精密度(n=6)均小于9%。

       

      Abstract: The sample (0.200 0 g) was extracted ultrasonically with ethanol for 30 min, and diluted to 10.0 mL with ethanol. The extract was separated by UHPLC using Zorbax SB-C18 column as stationary phase, and mixture of acetonitrile and 0.1% (φ) formic acid solution (17+3) as mobile phase. In MS analysis, ESI+ and MRM were adopted. Quantification was attained by external standard method with preparation of standard curves by matrix-matching method. As shown by the results, linear relationships between values of peak area and mass concentration of abietic acid and 11-carbonyl-β-acetyl boswellic acid were found in the same range of 10.0-1 000 μg·L-1, and the detection limits (3S/N) found were 0.9, 3.1 μg·kg-1 respectively. Test for recovery was made by standard addition method at 3 concentration levels, giving results in the range of 95.2%-101%. Values of the inter-and intra-day precision (RSDs, n=6) were all less than 9%.

       

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