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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王璐, 刘成雁, 王志嘉, 等. 超高效液相色谱-串联质谱法同时测定中药制剂中松香酸、11-羰基-β-乙酰乳香酸及苏丹红Ⅰ~Ⅳ的含量[J]. 分析测试学报, 2016,35(5):526-531.
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[J]. 2016,35(5):526-531.
王璐, 刘成雁, 王志嘉, 等. 超高效液相色谱-串联质谱法同时测定中药制剂中松香酸、11-羰基-β-乙酰乳香酸及苏丹红Ⅰ~Ⅳ的含量[J]. 分析测试学报, 2016,35(5):526-531. DOI:
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[J]. 2016,35(5):526-531. DOI:
建立了快速检测中药制剂中松香酸、11-羰基-β-乙酰乳香酸、苏丹红Ⅰ~Ⅳ的超高效液相色谱-串联质谱方法。样品以甲醇为提取溶剂,经Zorbax SB-C18色谱柱分离,以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,流速为0.3mL/min;采用电喷雾离子源(ESI),正离子多反应监测(MRM)扫描方式检测;基质匹配标准曲线法定量。结果表明,6种化合物分别在3.0~100μg/L(苏丹红Ⅰ,Ⅱ)及30~1000μg/L(松香酸、11-羰基-β-乙酰乳香酸及苏丹红Ⅲ,Ⅳ)范围内线性关系良好,相关系数均大于0.99,方法检出限为0.7~8.6μg?kg-1,定量下限为2.2~25.1μg?kg-1。低、中、高3个加标水平下各化合物的平均回收率为76.5%~94.9%,相对标准偏差(RSD)为2.3%~9.9%。采用酸化提取液的方法解决了苏丹红Ⅲ和Ⅳ的光学异构现象带来的计算误差。通过对目标化合物碎片离子的研究以及质谱裂解规律的总结,为其定性鉴别和定量分析提供了参考。该方法操作简便、准确、快速、灵敏,适合掺假中药制剂中松香酸及苏丹红含量的检测。
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.
超高效液相色谱-串联质谱法松香酸11-羰基-β-乙酰乳香酸苏丹红Ⅰ~Ⅳ中药制剂
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)abietic acidacetyl-11-keto-β-boswellic acidSudan Ⅰ-Ⅳtraditional Chinese medicine
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