摘要
目的:建立超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS)同时测定泽泻药材中16个主要成分(16-氧代泽泻醇A、16-氧代-24-乙酰泽泻醇A、泽泻醇C、泽泻醇F、23-乙酰泽泻醇C、11-去氧泽泻醇C、泽泻醇L、24-乙酰泽泻醇F、泽泻醇A、24-乙酰泽泻醇A、23-乙酰泽泻醇L、泽泻醇G、泽泻醇B、23-乙酰泽泻醇B、11-去氧泽泻醇B和11-去氧-23-乙酰泽泻醇B)的含量。方法:采用UPLC-MS/MS法,正离子多反应监测(MRM)模式进行含量测定。色谱条件:采用Cortecs C_(18)色谱柱(2.1 mm×100 mm,1.6μm),流动相为乙腈(A)-0.1%甲酸水溶液(B),梯度洗脱,流速0.25 mL·min^(-1),柱温40℃。结果:在所设定的色谱条件下,10 min内定量分析泽泻药材中上述16个主要成分,在考察的浓度范围内呈良好的线性关系(r>0.998 1),回收率和RSD分别在96.0%～104.3%和2.4%～4.4%范围内,精密度、重复性、稳定性考察也符合分析要求。24批样品中上述-16个成分含量测定结果依次为0.009～0.668 mg·g^(-1)、0.001～0.009 mg·g^(-1)、0.021～0.229 mg·g^(-1)、0.004～0.094 mg·g^(-1)、10.100～0.342 mg·g^(-1)、0.016～0.048 mg·g^(-1)、0.009～0.044 mg·g^(-1)、0.002～0.090 mg·g^(-1)、0.023～1.133 mg·g^(-1)、0.012～0.596 mg·g^(-1)、0.003～0.023 mg·g^(-1)、0～0.018 mg·g^(-1)、0.489～2.313 mg·g^(-1)、0.833～2.138 mg·g^(-1)、0.043～0.341 mg·g^(-1)、0.037～0.186 mg·g^(-1)。结论:本研究所建立的同时测定泽泻药材中16个成分的UPLC-MS/MS定量分析方法简便、快捷、准确,为泽泻药材质量控制提供新的技术手段。
Objective：To establish a UPLC-MS/MS method for simultaneous determination of 16 major components（16-oxo-alisol A,16-oxo-alisol A 24-actetate,alisol C,alisol F,alisol C23-acetate,11-deoxy-alisol C,alisol L,alisol F 24-actetate,alisol A,alisol A 24-acetate,alisol L 23-acetate,alisol G,alisol B,alisol B23-acetate,11-deoxy-alisol B and 11-deoxy-alisol B 23-acetate）in Alismatis Rhizoma. Methods：The UPLC-MS/MS assay was performed on a Waters Cortecs C_（18）（2.1 mm×100 mm,1.6 μm）column with acetonitrile-water（containing 0.1% formic acid）as mobile phase by gradient elution at a flow rate of 0.25 mL·min-1. The column temperature was set at 40℃. MS detection was performed with multiple reaction monitoring（MRM）mode using positive electrospray ionization. Results：Under the optimized chromatographic conditions,good separation for 16 target compounds was obtained within 10 min. Satisfactory linearity was achieved with wide linear range and fine determination coefficient（r0.998 1）,the recoveries were ranged from 96.0% to 104.3% with the RSDs within 2.4%-4.4%. Contents of the analytes in the samples were 0.009-0.668 mg·g-1,0.001-0.009 mg·g-1,0.021-0.229 mg·g-1,0.004-0.094 mg·g-1,0.100-0.342 mg·g-1,0.016-0.048 mg·g-1,0.009-0.044 mg·g-1,0.002-0.090 mg·g-1,0.023-1.133 mg·g-1,0.012-0.596 mg·g-1,0.003-0.023 mg·g-1,0-0.018 mg·g-1,0.489-2.313 mg·g-1,0.833-2.138 mg·g-1,0.043-0.341 mg·g-1 and 0.037-0.186 mg·g-1,respectively. Conclusion：The proposed UPLC-MS/MS method for simultaneous determination of 16 major components in Alismatis Rhizoma was simple,fast and accurate,which offered a new approach for quality control of Alismatis Rhizoma.
作者
邰艳妮
吴献
樊李明
吴照能
翁艳鸿
林青青
褚克丹
谢瑞华
TAI Yan-ni;WU Xian;FAN Li-ming;WU Zhao-neng;WENG Yan-hong;LIN Qing-qing;CHU Ke-dan;XIE Rui-hua(School of Pharmacy,Fujian University of Traditional Chinese Medicine,Fuzhou 350122,China;Fujian Chengtian Pharmaceutical Co.,Ltd.,Nanping 354099,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第8期1337-1350,共14页
Chinese Journal of Pharmaceutical Analysis
基金
国家中医药管理局项目(ZYBZH-Y-FJ-09)
作者简介
Tel：18344980445：E—mail：1151545049@qq．com;通信作者林青青Tel：（0591）22861216；E-mail：54823860@qq．com;通信作者褚克丹Tel：（0591）22861661；E—mail：chukd5917@163．com
