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
步献功 1李孟璇 1牛悦齐 2齐鹤鸣 3张勋 2李志远 4邹明强 5魏冬旭 6胡婷婷2
作者信息
- 1. 长春海关技术中心,长春 130062;吉林大学公共卫生学院,长春 130000
- 2. 长春海关技术中心,长春 130062
- 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
- 折叠
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.
Abstract
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Key words
high performance liquid chromatography-time-of-fight mass spectrometry/health food/drugs引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据