摘要
目的:建立减肥类中成药和保健食品非法添加胡椒碱的超高效液相色谱-紫外光谱-飞行时间质谱(UPLC-DAD-ESI-Q-TOF/MS)检验方法。方法:样品采用甲醇超声提取,经ACQUITY UPLC;HSS T3(100 mm×2.1 mm,1.8μm)色谱柱分离,以0.1%甲酸溶液和0.1%甲酸-乙腈梯度洗脱,流速为0.3 ml·min^(-1)。采用电喷雾离子源正离子模式(ESI^(+)),利用Q-TOF一级精密质量数建立含量测定方法,保留时间、紫外吸收光谱和二级质谱碎片用于进一步定性确证。结果:在本方法条件下,胡椒碱在7 min内获得良好的分离效果;在0.5~10μg·ml^(-1)浓度范围内,线性关系良好(r>0.990);回收率为95.0%~109.1%;RSD小于4%。当取样量为1 g,稀释倍数为100时,检出浓度为0.51 mg·kg^(-1),定量浓度为1.7mg·kg^(-1)。结论:本方法可专属、灵敏、快速地初筛并确证减肥类中成药和保健食品中非法添加的胡椒碱,主要适用于片剂、胶囊剂型中胡椒碱的分析。
Objective:To establish a UPLC-DAD-ESI-Q-TOF/MS method for the identification of piperine,a new additive in slimming traditional Chinese medicine and health foods.Methods:The samples were extracted by methanol in an ultrasonic machine methanol,and the separation was performed on an ACQUITY UPLC;HSS T3 column with a mobile phase consisting of 0.1%formic acid(A)and 0.1%formic acid-acetonitrile(B)at a flow rate of 0.3 ml·min^(-1).Electro spray ionization source in positive ion mode was applied to mass spectrometry,and the data used for precise quantification were collected by using a full mass scan mode.The confirmatory analysis for target compounds was performed with the retention time,ultra-violet spectrum and MS;scan.Results:Under the conditions of this method,piperine obtained a good separation effect within 7 minutes;within the concentration range of 0.5-10μg·ml^(-1),the linear relationship was good(r>0.990);the recovery was 95.0%-109.1%;the relative standard deviation was less than 4%.When the sampling amount was 1 g and the dilution ratio was 100,the detection concentration was 0.51 mg·kg^(-1) and the quantitative concentration was 1.7 mg·kg^(-1).Conclusion:This method can be used exclusively,sensitively and quickly to screen and confirm piperine added to slimming traditional Chinese medicine and health foods.It is mainly suitable for the analysis of piperine in tablets and capsules.
作者
张珊珊
张萍
闵春艳
陈卫
贾昌平
Zhang Shanshan;Zhang Ping;Min Chunyan;Chen Wei;Jia Changping(Suzhou Institute for Drug Control,Jiangsu Suzhou 215104,China;Wuhu Institute for Food and Drug Control)
出处
《中国药师》
CAS
2022年第1期194-197,共4页
China Pharmacist
基金
安徽省药品监督管理局科技创新项目(编号:AHYJ-KJ-202012)。
