保健食品中可能添加的毒品快速检测技术研究  

Study on Rapid Detection Technology of Drugs that May Be Added in Health Food

作　　者：步献功 李孟璇 牛悦齐 齐鹤鸣 张勋 李志远 邹明强[5] 魏冬旭 胡婷婷 Bu Xiangong;Li Mengxuan;Niu Yueqi;Qi Heming;Zhang Xun;Li Zhiyuan;Zhou Mingqiang;Wei Dongxu;HU Tingting(Changchun Customs Technology Center,Changchun 130062,China;Jilin University,School of Public Health Changchun 130000,China;Science and Technology Research Center of China Customs,Beijing 100026,China;Shanghai AB Sciex Analytical Instrument Trading Co.,Ltd,Beijing 100015;China Academy of inspection and quarantine Sciences,Beijing 100176,China;Haerbin Customs Technology Center,Haerbin 150000)

机构地区：[1]长春海关技术中心,长春130062 [2]吉林大学公共卫生学院,长春130000 [3]中国海关科学技术研究中心,北京100026 [4]上海爱博才思分析仪器贸易有限公司,北京100015 [5]中国检验检疫科学研究院,北京100176 [6]哈尔滨海关技术中心,哈尔滨150000

出　　处：《现代科学仪器》2024年第5期33-39,共7页Modern Scientific Instruments

基　　金：吉林省科技发展计划项目(重点研发项目)20210203045SF;海关总署科研项目2020HK182;中国海关科学技术研究中心研课题2023HX07;长春海关科技项目CCHG2023KY04。

摘　　要：建立了基于高效液相色谱-高分辨飞行时间质谱联用技术(HPLC-TOF/MS)快速定性确证及定量检测保健食品中可能添加的22种毒品的分析方法。样品用乙腈提取,亲水亲脂HLB固相萃取柱净化,经Phenomenex Kinetex F5五氟苯基色谱柱(100mm×3.0mm,2.6μm)分离,用含0.1%甲酸5mmol·L^(-1)甲酸铵水溶液,5mmol·L^(-1)甲酸铵乙腈溶液为流动相,HPLC-TOF/MS检测,外标法定量。22种毒品在各自线性范围内均有较好的线性关系,回归系数R2>0.9990。方法的检出限在0.2~2.0ng·g^(-1)之间,阴性样品(片剂、胶囊、液体、软胶囊)中,添加水平分别为5、10、20ng·g^(-1)的加标平均回收率在62.33%~110.82%之间,测定结果的相对标准偏差在1.18%~10.52%之间。该方法前处理简单,检测快速,适用范围广,灵敏度和准确度符合要求,适用于检测保健食品中可能添加的多种毒品。An analytical method based on high performance liquid chromatography-high resolution time-of-flight mass spectrometry(HPLC-TOF/MS)was established for the qualitative and quantitative detection of 22 drugs that may be added to health food.The samples were extracted with acetonitrile,purified by HLB solid phase extraction column,separated by Phenomenex Kinetex F5 pentafluorophenyl column(100 mm×3.0mm,2.6μm)5 mmol·L^(-1)ammonium formate 0.1%formic acid aqueous solution,5 mmol·L^(-1)ammonium formate acetonitrile solution as mobile phase,detected by HPLC-TOF/MS,and quantified by external standard method.22 kinds of drugs in their respective linear range show a good linear relationship,the regression coefficient R2>0.9990.The limits of detection(LOD)for the 22 drugsare in the range of 0.2~2.0ng·g^(-1).The average recoveries of negative samples(tablets,capsules,liquids,soft capsules)at the spiked levels of 5,10,20 ng·g^(-1)are between 62.33%and 110.82%,and the relative standard deviations of the determination results were between 1.18%and 10.52%.The method has the advantagesof simply previous treatment process,shorter detection time,wide range of application,good sensitivity and accuracy,and is suitable for the detection of various drugs that may be added in health food.

关 键 词：高效液相色谱-高分辨飞行时间质谱 保健食品 毒品 

分 类 号：O65[理学—分析化学]