UPLC-QTRAP-MS/MS检测保健食品中非法添加伪品大黄及其提取物  

Determination of fake Rhei Radix et Rhizoma and its extract in health food by UPLC-QTRAP-MS/MS

作　　者：段琼 马春艳 曹春琪 高晋梅 孟珊 封淑华 DUAN Qiong;MA Chun-yan;CAO Chun-qi;GAO Jin-mei;MENG Shan;FENG Shu-hua(Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050200,China;Hebei University of Science and Technology,Shijiazhuang 050018,China)

机构地区：[1]河北省药品医疗器械检验研究院,石家庄050200 [2]河北科技大学,石家庄050018

出　　处：《药物分析杂志》2021年第12期2171-2177,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：河北省食品药品监督管理局重点科技项目(ZD2014006);2021年度河北省市场监督管理局科技项目(2021YJ05)。

摘　　要：目的:建立以土大黄苷为标志性成分的保健食品中非法添加伪品大黄及其提取物的UPLC-QTRAP-MS/MS的分析方法。方法:样品用甲醇经超声提取,经Agilent InfinityLab Poroshell 120 SB-C_(18)色谱柱(100 mm×2.1 mm,2.7μm)分离,以5 mmol·L^(-1)甲酸铵水溶液和乙腈作为流动相,进行梯度洗脱,在负离子扫描模式下,采用MRM-IDA-EPI模式检测。结果:土大黄苷质量浓度在5~100 ng·mL^(-1)范围内线性均良好。相关系数(r^(2))为0.9987。土大黄苷在1.25、2.5和12.5 mg·kg^(-1)水平下,茶、胶囊、片剂、颗粒剂、液体五种基质中的加标回收率为86.3%~118.7%。对市场抽检获得的18批相关样品进行了测定,结果有1批次检出土大黄苷,含量约为表明其样品中掺入伪品大黄。结论:本方法简单、快速、可靠,灵敏度高,可满足保健食品市场的监管和检验需求。Objective:To develop an analytical method with rhapontin as the marker for fake Rhei Radix et Rhizoma and its extract added in health food by UPLC-QTRAP-MS/MS.Methods:The sample was extracted by menthol with ultrasound extraction and then separated on Agilent Infinity Lab Poroshell 120 SB-C_(18)(100 mm×2.1 mm,2.7μm)column with gradient elution.The mobile phase consisted of 5 mmol·L^(-1)HCOONH_(4) in water and acetonitrile.Negative MRM-IDA-EPI was used to quantify and identify the target.Results:The linear relationship was good in the range of 5-100 ng·mL^(-1),and the correlation coefficient(r^(2))was 0.9987.Theaverage recovery at 1.25 mg·kg^(-1),2.5 mg·kg^(-1)and 12.5 mg·kg^(-1)levels were 86.3%-118.7%in five base materials including tea,capsule,tablet,granule and liquid.One of the 18 batches of the samples collected was detected fake Rhei Radix et Rhizoma and its extract.Conclusion:The method is accurate,sensitive,specific with low detection limit.It can be used for the qualitative and quantitative determination in slimming health foods.

关 键 词：保健食品 添加 土大黄苷 伪品大黄 超高效液相色谱-三重四极杆/线性离子阱 多反应监测-增强子离子扫描 

分 类 号：R917[医药卫生—药物分析学]