首页|固相萃取-超高效液相色谱-串联质谱法测定六神曲中4种烷基间苯二酚

固相萃取-超高效液相色谱-串联质谱法测定六神曲中4种烷基间苯二酚

Determination of 4 Alkylresorcinols in Massa Medicata Fermentata by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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建立固相萃取-超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定六神曲中5-十五烷基间苯二酚(AR-15)、5-十七烷基间苯二酚(AR-17)、5-十九烷基间苯二酚(AR-19)和5-二十一烷基间苯二酚(AR-21)4种烷基间苯二酚含量.分析采用Brownless Spp C18色谱柱(2.1mm×100mm,2.7μm),流动相:A相为5mmol/L乙酸铵溶液,B相为甲酸:乙腈溶液(体积比为1︰1000),采用梯度洗脱方式,体积流速为0.5Ml/min.柱温为35℃,使用电喷雾离子源,负离子扫描,多反应监测模式.结合主成分分析与正交偏最小二乘法判别分析,寻找影响六神曲炮制前后质量的主要化学成分.结果表明,4种成分在各自范围内线性关系良好(r>0.9926),平均加样回收率在99.36%~101.36%之间,相对标准偏差(RSD)为0.85%~2.10%.通过化学模式识别分析发现造成主要差异的质量差异物是AR-21.方法简便可行,稳定可靠,可用于炮制不同六神曲的质量控制.
A method of solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been established for the simultaneous determination of 4 alkylresorcinols in Massa Medicata Fermentata,including 5-pentadecyl resorcinol (AR-15),5-heptadecylresorcinol (AR-17),5-nonadecylresorcinol (AR-19)and 5-heneicosylresorcino (AR-21). The analysis was performed on a Brownless Spp C18 column (2.1 mm×100 mm,2.7μm) with the mobile phase of 5 mmol/L ammonium acetate solution in phase A and formic acid:acetonitrile solution (volume ratio of 1∶1000) in phase B at a flow rate of 0.5 mL/min with gradient elution. The column temperature was 35 ℃,and the electron spray ionization source was adopted in negative ion scanning with multiple reaction monitoring mode. Combined with principal component analysis and orthogonal partial least square-discriminant analysis,the main chemical components affecting the quality of Massa Medicata Fermentata before and after processing were found. The results showed that 4 components had good linear relationships in their respective ranges (r>0.9926),the average spiked recoveries ranged from 99.36% to 101.36%,and the relative standard deviations (RSD) were 0.85%~2.10%. The mass difference substance was AR-21 that caused the main difference through chemical pattern recognition analysis. The method is simple,feasible,stable and reliable,and can be used for the quality control of different products of Massa Medicata Fermentata.

Massa Medicata Fermentataalkylresorcinolsolid phase extractionUPLC-MS/MS

李运、刘晓玲、许晓辉、王苗、李红玉

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兰州市食品药品检验检测研究院/甘肃省种植中药材外源性污染物监测工程研究中心,兰州 730050

兰州大学药学院,兰州 730000

甘肃中医药大学药学院,兰州 730000

六神曲 烷基间苯二酚 固相萃取 超高效液相色谱-串联质谱法

甘肃省药品科研项目陇原青年创新创业人才项目兰州市青年科技人才创新项目

2022GSMPA00372023LQGR492023-QN-144

2024

分析测试技术与仪器
中国科学院兰州化学物理研究所,中国科学院计划财务局,中国科学院兰州分院分析测试中心

分析测试技术与仪器

影响因子:0.444
ISSN:1006-3757
年,卷(期):2024.30(4)