摘要
建立一种检测降血压、降血脂和降血糖类保健食品中58种非法添加药物的高效液相色谱-高分辨质谱分析方法。样品经酸化乙腈提取,采用基于QuEChERS原则的快速净化技术,以0.1%甲酸-5 mmol/L甲酸铵水溶液和甲醇-乙腈(体积比为1∶1)为流动相,进行梯度洗脱,经ESI正模式扫描,建立了包括58种药物的结构信息、一级/二级精确质量数等在内的数据谱库,用于未知样品二级质谱图自动匹配确证。保健食品中58种非法添加物可同时进行定性及定量检测,线性关系良好,相关系数不小于0.999 0,检出限为0.01~10 ng/mL,定量限为0.03~30 ng/mL。平均回收率为64.25%~115.3%,相对标准偏差为1.1%~17.85%(n=6)。该方法样品处理简单,灵敏度高,特异性强,可为保健品中降三高类非法添加物质的高通量筛查确证提供方法参考。
A method for the determination of 58 illegally added antihypertensive drugs,antihyperlipidemic drugs and hypoglycemic drugs in health care food by high performance liquid chromatography-high resolution mass spectrometry was established.Samples were extracted by acidified acetonitrile and purified based on the QuEChERS principle.0.1%formic acid-5 mmol/L ammonium formate aqueous solution and methanol-acetonitrile(volume ratio of 1∶1)were used as mobile phases for gradient elution.The electrospray positive ionization scanning mode was used for detection,the chemical structure information and primary/secondary accurate mass spectrometry were collected to construct a data spectrum library for 58 illegally added chemicals.It could be used for automatic matching and confirmation of secondary mass spectra of unknown samples.The method could simultaneously detects 58 illegally added chemicals in health care foods,with a good linear relationship and the correlation coefficients of all more than 0.9990.The detection limits were 0.01-10 ng/mL,and the quantitative limits were 0.03-30 ng/mL.The average recoveries were 64.25%-115.3%,and the relative standard deviations were 1.1%-17.85%(n=6).The method has simple pretreatment,high sensitivity and strong specificity,which provides a high throughput qualitative screening and confirmation method for illegally added chemicals of reduce three highs class in health care foods.
作者
李孟璇
步献功
杜佳剑
马书民
张勋
董昕
李志远
梁多
胡婷婷
LI Mengxuan;BU Xiangong;DU Jiajian;MA Shumin;ZHANG Xun;DONG Xin;LI Zhiyuan;LIANG Duo;HU Tingting(Changchun Customs Technology Center,Changchun 130062,China;Jilin University School of Public Health,Changchun 130000,China;Shanghai AB Sciex Analytical Instrument Trading Co.,Ltd.,Bei Jing 100015,China)
出处
《化学分析计量》
CAS
2024年第5期48-59,共12页
Chemical Analysis And Meterage
基金
吉林省科技发展计划项目(20210203045SF)
长春海关关级项目(CCHG2023KY11)
海关总署科研项目(2020HK182)。
关键词
高效液相色谱-高分辨质谱法
降血压
降血脂
降血糖
非法添加
保健食品
high performance liquid chromatography-high resolution mass spectrometry
antihypertensive
antihyperlipidemic
hypoglycemic
illegally added
health care foods
作者简介
通信作者:胡婷婷,博士,正高级工程师,研究方向为食品检验。
