分散固相萃取-超高效液相色谱-质谱法检测保健茶中6种利尿类兴奋剂  

Determination of six diuretics in health teas by DSPE-UPLC-MS/MS

作　　者：李涛 杨庆懿 王亮亮 周艳华[2] 李政 LI Tao;YANG Qingyi;WANG Liangliang;ZHOU Yanhua;LI Zheng(Hunan Institute of Commodity Quality Inspection,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410111;Changsha Environmental Protection College,Changsha 410004)

机构地区：[1]湖南省产商品质量检验研究院,食品安全监测与预警湖南省重点实验室,长沙410111 [2]长沙环境保护职业技术学院,长沙410004

出　　处：《中国食品添加剂》2025年第4期108-113,共6页China Food Additives

基　　金：湖南省自然科学基金(编号:2022JJ90027);湖南省自然科学基金项目(编号:2023JJ60533)。

摘　　要：为了建立分散固相萃取结合超高效液相色谱—串联质谱法(UPLC-MS/MS)检测保健茶中6种利尿类兴奋剂的方法。样品经乙腈提取,C18和HLB萃取剂组合净化后,经C18色谱柱(50 mm×2.1 mm,3.0μm)分离,0.1%甲酸(体积分数)甲酸铵溶液(5 mmol/L)-乙腈为流动相,梯度洗脱,正离子模式下检测分析,外标法定量。结果显示:6种利尿剂在1.0~100.0 ng/mL范围内呈良好的线性关系,相关系数>0.996。检出限均为0.6μg/kg,定量限均为2.0μg/kg。在加标浓度为2.0~20.0μg/kg,6种利尿剂加标回收率在78.3%~98.3%范围内,RSD在2.7%~8.7%范围内。对市场采购20批次保健茶进行检测,所有样品均未检出。该法简单高效、灵敏度高、选择性强,可作为保健茶中6种利尿剂检测方法。A method was established for the detection of 6 diuretics in health teas by dispersion solid-phase extraction combined with ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).The samples were extracted by acetonitrile and purified by combination of C18 and HLB extractants,then separated on C18(50 mm×2.1 mm,3.0μm)column with 0.1%formic acid(v/v)ammonium formate solution(5 mmol/L)-acetonitrile for gradient elution.The compound was detected and analyzed in the positive ion mode,and quantified by the external standard method.The results demonstrated that the six diuretics exhibited a good linear relationship within the range of 1.0 to 100.0 ng/mL,with correlation coefficients exceeding 0.996.The limits of detection were all found to be 0.6μg/kg,while the limits of quantification were set at 2.0μg/kg.When spiked at concentrations ranging from 2.0 to 20.0μg/kg,the recovery rates for the six diuretics ranged from 78.3%to 98.3%,with relative standard deviations(RSDs)between 2.7%and 8.7%.Testing was conducted on 20 batches of health teas purchased from the market,and all samples tested negative for the diuretics.This method was simple,efficient,highly sensitive,and highly selective.It can be used as a method for the determination of 6 diuretics in health teas.

关 键 词：利尿剂 分散固相萃取 保健茶 方法学 超高效液相色谱串联质谱法 

分 类 号：TS202.1[轻工技术与工程—食品科学] O65[轻工技术与工程—食品科学与工程]