保健食品中可能添加的毒品快速检测技术研究OACSTPCD
Study on Rapid Detection Technology of Drugs that May Be Added in Health Food
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.
步献功;李孟璇;牛悦齐;齐鹤鸣;张勋;李志远;邹明强;魏冬旭;胡婷婷
长春海关技术中心,长春 130062||吉林大学公共卫生学院,长春 130000长春海关技术中心,长春 130062||吉林大学公共卫生学院,长春 130000长春海关技术中心,长春 130062中国海关科学技术研究中心,北京 100026长春海关技术中心,长春 130062上海爱博才思分析仪器贸易有限公司,北京 100015中国检验检疫科学研究院,北京 100176哈尔滨海关技术中心,哈尔滨 150000长春海关技术中心,长春 130062
化学
高效液相色谱-高分辨飞行时间质谱保健食品毒品
high performance liquid chromatography-time-of-fight mass spectrometryhealth fooddrugs
《现代科学仪器》 2024 (5)
33-39,7
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.
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