摘要
目的建立高效液相色谱-离子阱质谱法同时检测芦荟保健食品中蒽醌类成分芦荟苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚及7种常见非法添加减肥化学药物的测定方法。方法采用Waters XBridge C18柱(4.6 mm×250 mm,5μm),以0.02 mol/L乙酸铵溶液(含0.05%乙酸)(A)-甲醇(B)为流动相,梯度洗脱,流速为1.0 ml/min,柱温为30℃,检测波长为225 nm。质谱条件:扫描方式:正、负离子同时扫描;雾化气压:35 psi,去溶剂气温度:350℃,去溶剂气流量:10 L/min;离子扫描范围:m/z 80-m/z 800;通过比较供试品与对照品一级和二级质谱,对样品中蒽醌类成分及非法添加的化学药物进行定性鉴别,同时用所建立的液相方法对13种化学物质进行定量分析。结果13种化合物标准曲线线性关系良好,所有化合物的线性相关系数(r)都>0.995,检出限均低于0.2μg/ml,各化合物回收率在85%~105%,相对标准偏差<4%。结论方法简便、快速、灵敏、准确,适于芦荟类保健食品中目标含量及非法添加化学药物的测定。
Objective To establish a method for the determination of barbaloin aloe-emodin, rhein, emodin, chrysophanol, physcion and seven familar illegal addition of weight loss chemicals in aloe health food by liquid chromatography-ion trap tandem mass spectrometry. Methods The sample was separated on a Waters XBridge C18(4.6 mm×250 mm, 5 μm) column with a mobile phase consisting of 0.02 mol/L ammonium acetate solution(containing 0.05% acetic acid)(A)-methanol(B) for gradient elute solution, the flow rate was 1.0 ml/min, and the column temperature was set at 30 ℃ and determination wavelength was 225 nm. Mass spectrometry conditions were as the following: scanning mode was set at simultaneous scanning of positive and negative ions, atomizing air pressure was 35 psi, solvent removal temperature was 350 ℃, desolvation gas flow was 10 L/min, ion scanning range was within 80 m/z-800 m/z;compared with mass spectrogram, qualitative identification of anthraquinones and illegally added chemicals in aloe health food and 13 chemical substances were quantitatively analyzed by the established liquid phase method. Results The validated method indicated that the correlation coefficients(r) for all elements were above 0.995. The detection limits were under 0.2 μg/mL. The recovery rates of the elements were within 85%-105%, with RSD less than 4%. Conclusion The proposed method was simple, fast, sensitive and accurate, which was suitable for the determination of target content and other chemicals in aloe health food.
作者
徐慧
郭小鹏
王超
杨钊
XU Hui;GUO Xiao-peng;WANG Chao;YANG Zhao(Qingdao Institute for Drug and Food Control,Qingdao,Shandong 266071,China;不详)
出处
《中国卫生检验杂志》
CAS
2019年第22期2703-2706,共4页
Chinese Journal of Health Laboratory Technology
关键词
芦荟保健食品
高效液相色谱-离子阱质谱法
蒽醌
非法添加化学药物
Aloe health food
Liquid chromatography-ion trap tandem mass spectrometry
Anthraquinone
Illegally added chemicals
