超高效液相色谱-串联质谱法对癍痧凉茶中18种活性成分的定量分析  

Quantitative Analysis of 18 Active Components in Bansha Herbal Tea by Ultra High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

作　　者：梁慧[1] 朱伟健[1] 袁智泉[2] 陈超[1] 吴庆晖[1] 杨运云[1] 

机构地区：[1]中国广州分析测试中心广东省化学危害应急检测技术重点实验室,广东广州510070 [2]安捷伦科技有限公司安捷伦-中广测联合技术中心,广东广州510070

出　　处：《分析测试学报》2015年第5期558-563,569,共7页Journal of Instrumental Analysis

基　　金：广东省科技计划重点项目(2010A030100013)

摘　　要：建立了超高效液相色谱-串联质谱（UHPLC-MS/MS）测定癍痧凉茶中18种活性成分的定量分析方法。癍痧凉茶样品经甲醇萃取后,采用RRHD SB-C18（100 mm×3.0 mm,1.8μm）超高效液相色谱柱进行分离,以0.5%甲酸水溶液-乙腈为流动相进行梯度洗脱。18种活性成分的定量分析采用三重四极杆串联质谱以负离子检测模式多重反应离子监测进行。实验结果表明,所建立的方法线性良好,18种目标化合物的线性相关系数（r）不小于0.996 4;分析方法的灵敏度高,检出限和定量下限分别为0.001~0.08μg/m L和0.002~0.27μg/m L;同时具备精密度高、准确度好、稳定性理想等优点。建立的分析方法用于测定11批＂黄振龙＂癍痧凉茶和8批＂平安堂＂凉茶。结果表明,＂黄振龙＂和＂平安堂＂样品中18种活性成分的浓度分别为0.7~149.8μg/m L和0.9~110.3μg/m L。采用主成分分析（PCA）对这19批次癍痧凉茶样品进行来源追踪,并对其质量的稳定性和一致性进行了评价。PCA得分图可将两个厂家的癍痧凉茶明显区分开,提示两种凉茶的配方组成及生产工艺不同,所建立的分析方法可有效用于癍痧凉茶的质量评价与控制。A method for the quantitative analysis of 18 active components in Bansha herbal tea（ BHT）by ultra high performance liquid chromatography coupled with tandem mass spectrometry（ UHPLC-MS / MS） was developed. BHT samples were extracted with methanol,and the extracts were separated on an RRHD SB-C18 column with 0. 5% formic acid aqueous solution-acetonitrile as mobile phase by gradient elution. Quantitative analysis was performed by a triple quadrupole MS system operated under multiple-reaction monitoring（ MRM） mode in negative ion detection mode. The method showed a good linearity with correlation coefficients（ r） not less than 0. 996 4 for 18 investigated analytes. The limits of detection and quantitation were in the ranges of 0. 001-0. 08 μg / m L and 0. 002-0. 27 μg / m L,respectively. In addition,high precision,good accuracy,and desirable stability were also obtained. The developed method was then used for the determination of the contents of 18 active components in 11 Huangzhenlong（ HZL） and 8 Pingantang（ PAT） BHT samples. The results showed that the concentrations of 18 investigated active components ranged from 0. 7 to 149. 8 μg / m L and 0. 9to 110. 3 μg / m L for HZL and PAT samples,respectively. Principal component analysis（ PCA） was performed to evaluate the quality stability and consistency and trace the origins of the 19 batches of investigated BHT samples. PCA results showed that two manufactures BHT samples were easy to differentiate by using the PCA score plot,indicating that the formulas and the production processes of the two BHT products were different. The proposed method was a desirable approach for the quality assessment and control of BHT.

关 键 词：超高效液相色谱-串联质谱 癍痧凉茶 活性成分 定量分析 

分 类 号：O657.6[理学—分析化学] R961.1[理学—化学]