Simultaneous Determination of Abietic Acid,Acetyl-11-keto-β-boswellic Acid and Sudan Ⅰ-Ⅳ in Traditional Chinese Medicine by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
  
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KeyWord:ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  abietic acid  acetyl-11-keto-β-boswellic acid  Sudan Ⅰ-Ⅳ  traditional Chinese medicine
  
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WANG Lu,LIU Cheng-yan,WANG Zhi-jia,REN Xue-dong,WU Dong-dong,YOU Hai-dan,XIONG Shuang 辽宁省分析科学研究院辽宁省标准化体系建设工程技术研究中心辽宁省分析测试技术研究重点实验室
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Abstract:
      An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the simultaneous determination of abietic acid,acetyl-11-keto-β-boswellic acid and Sudan Ⅰ-Ⅳ in traditional Chinese medicine.The sample was extracted with methanol,and then separated on a Zorbax SB-C18(3.5μm,2.1mm×150mm) chromatographic column using a mixture of acetonitrile and 0.1% formic as mobile phase by gradient elution at a flow rate of 0.3mL/min.The electrospray was operated in the positive mode under the multiple reaction monitoring(MRM) mode,and the quantitation was carried out by the matrix standard curve.As a result,the calibration curves for Sudan Ⅰ/Ⅱ were linear in the range of 3.0-100μg/L,and for the others were linear in the range of 30-1000μg/L.The correlation coefficients for all the compounds were greater than 0.99.The limits of detection(LOD) ranged from 0.7μg?kg-1 to 8.6μg?kg-1,and the limits of quantitation(LOQ) ranged from 2.2μg?kg-1 to 25.1μg?kg-1.The average recoveries of six compounds at three spiked levels were in the range of 76.5%-94.9% with relative standard deviations(RSD) of 2.3%-9.9%.It was demonstrated that the first peak would not appear if the sample was kept in methanol-5% formic acid solution which could be avoided 10% errors in quantitative analysis for Sudan Ⅲ and Sudan Ⅳ. Moreover, the mass spectrometric behaviour and the ion fragmentation patterns of six compounds could provide beneficial references for the qualitative identification and quantitative analysis.This method is simple,rapid and accurate,and is suitable for the rapid determination of abietic acid,acetyl-11-keto-β-boswellic acid and Sudan Ⅰ-Ⅳ in traditional Chinese medicine.
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