Comparison of microwave-assisted and heat reflux extraction techniques for the extraction of ten major compounds from Zibu Piyin Recipe using ultra high performance liquid chromatography with tandem mass spectrometry.
Comparison of microwave-assisted and heat reflux extraction techniques for the extraction of ten major compounds from Zibu Piyin Recipe using ultra high performance liquid chromatography with tandem mass spectrometry.
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DOI：
10.1002/jssc.201501033
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发表时间：
2016-03
影响因子：
3.1
通讯作者：
Huiying Xu;Libin Zhan;Lin Zhang
中科院分区：
文献类型：
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作者：
Huiying Xu;Libin Zhan;Lin Zhang
采用微波辅助提取和高效超高效液相色谱-三重四极杆质谱法同时快速提取和定量测定滋补脾阴方中人参皂苷Rf、Ro、Rd、20(R)-人参皂苷-Rg2、20(R)-人参皂苷-Rg2、丹参酮IIA、隐丹参酮、二氢丹参酮I、石精酸、蛇床子素。我们在这里表明，热回流提取这些目标化合物的效率更高，但更耗时。色谱柱为Agilent ZORBAX RRHD Eclipse Plus C18色谱柱，流动相为水/0.5%甲酸-乙腈，流速为0.2mL/min，检测采用正负离子多反应监测模式。所有分析物在检测范围内均呈良好的线性关系(r=0.9989~0.9999)，检出限为0.002~0.180μg/mL。10种化合物的日内和日间变异系数(≤)为2.9%，精密度为97.61-103.18%(≤4.25%)。分析结果表明，微波辅助提取法和热回流提取法提取的滋补脾阴方中10种化合物的含量有显著差异。这些结果为确定滋补脾阴方的质量提供了重要信息。
Microwave-assisted extraction and efficient ultra-high performance liquid chromatography with triple quadrupole mass spectrometry were previously used to quickly extract and simultaneously quantify ginsenoside Rf, Ro, and Rd, 20(S)-ginsenoside-Rg2 , 20(R)-ginsenoside-Rg2 , tanshinone IIA, cryptotanshinone, dihydrotanshinone I, lithospermic acid, and osthole from Zibu Piyin Recipe. We here showed that heat reflux extraction provides higher extraction efficiency of these target compounds but is more time consuming. Chromatographic separation was achieved on an Agilent ZORBAX RRHD Eclipse Plus C18 column with a gradient mobile phase consisting of water/0.5% formic acid and acetonitrile at a flow rate of 0.2 mL/min, and detection was performed by positive and negative ion multiple-reaction monitoring mode. All analytes showed good linearity (r, 0.9989-0.9999) within the test range, with a limit of detection of 0.002-0.180 μg/mL. The overall intra- and interday variations of the ten compounds were ≤2.9%, and the accuracy was evaluated using a recovery test at three concentrations and was in the range 97.61-103.18% (RSD ≤ 4.25%). The analytical results showed remarkable differences in the concentrations of the ten compounds extracted from Zibu Piyin Recipe by microwave-assisted extraction and heat reflux extraction. These findings provide important information for determining the quality of Zibu Piyin Recipe.