摘要
针对保健食品中的双醋酚丁、托拉塞米和脱乙酰比沙可定,建立了一种基于QuEChERS前处理与液相色谱-串联质谱(liquid chromatography-mass spectrometry/mass spectrometry,LC-MS/MS)联用的检测方法。样品经乙腈提取、QuEChERS吸附剂净化后,将样品溶液引入LC-MS/MS进行分析,在多反应监测模式下检测。该方法针对3种目标分析物的检出限为0.002 mg/kg,定量限为0.010 mg/kg。采用所建立的方法对市售的片剂、粉剂、口服液、胶囊剂、煎膏剂和丸剂类型保健食品中双醋酚丁、托拉塞米和脱乙酰比沙可定进行了检测,样品均未检出目标分析物。对片剂、粉剂、口服液、胶囊剂、煎膏剂和丸剂进行加标回收试验,回收率在86.8%~108%之间,精密度为5.2%~12.0%(c=0.010 mg/kg,0.020 mg/kg,0.100 mg/kg,n=7)。这表明所建立的方法快速、简便、易于批量操作且具有良好的准确性,可满足保健食品中双醋酚丁、托拉塞米和脱乙酰比沙可定的测定。
A method based on QuEChERS pretreatment combined with liquid chromatography-mass spectrometry/mass spectrometry(LC-MS/MS)was established for the determination of diaotyldiphenolisatinum,torasemide and deacetylbisacodyl in health foods.The samples were subjected to the extraction of acetonitrile and puriffcation of QuEChERS sorbents,and the extraction solution was then introduced into LC-MS/MS for multiple reaction monitoring(MRM)detection.The detection limit of the method for the three target analytes was 0.002 mg/kg,and the quantiffcation limit was 0.010 mg/kg.The established method was used to detect diaotyldiphenolisatinum,torasemide and deacetylbisacodyl in commercially available tablets,powders,oral liquids,capsules,extracts,and pill-type health foods,and no target analytes were detected in the samples.For tablets,powders,oral liquids,capsules,extracts,and pills,the recovery rates of the spike recovery test were between 86.8%-108%,and the precision was between 5.2%-12.0%(c=0.010 mg/kg,0.020 mg/kg,0.100 mg/kg,n=7).This indicates that the established method is rapid,simple,easy to batch operate,and has good accuracy,and can satisfy the determination of diaotyldiphenolisatinum,torasemide and deacetylbisacodyl in health foods.
作者
王晗
杨青
万莹
赵晓亚
尚吟竹
王惠
王鹏
WANG Han;YANG Qing;WAN Ying;ZHAO Xiao-Ya;SHANG Yin-Zhu;WANG Hui;WANG Peng(Wuhan Customs Technology Center,Wuhan 430000)
出处
《中国口岸科学技术》
2023年第7期47-55,共9页
China Port Science and Technology
