摘要
【目的】建立超高效液相色谱⁃四极杆飞行时间质谱定性测定食品中52种减肥类非法食品添加物的方法。【方法】以甲醇超声提取样品,采用Waters CORTECS T3色谱柱(100 mm×2.1 mm,2.7µm),以0.1%甲酸溶液⁃乙腈为流动相进行梯度洗脱,采用电喷雾离子(ESI)源,Q⁃TOF⁃MS作检测器,正、负离子模式检测。以标准品建立标准谱库,供试品与标准谱库中各化合物的保留时间、母离子及碎片离子精确相对分子质量进行比对,准确定性。【结果】该方法专属性好,空白基质无干扰;重复性好,一式6份均可检出;52种化合物在5种基质中检出限为1~100 mg‧kg^(−1)。方法已应用于实际样品测定中,246批样品中共检出16种化合物。【结论】该方法定性准确、专属灵敏,可有效打击减肥类食品中的非法添加行为。
[Objective]An analytical method was developed for the qualitative screening of 52 illegally adulterated weight-losing compounds in foods by ultra high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry.[Methods]The samples were extracted by methanol.Waters CORTECS T3 column(100 mm×2.1 mm,2.7µm)was used with acetonitrile−0.1%formic acid aqueous solution as mobile phases by gradient elution.The compounds were detected by electrospray ionization mass spectrometry and Q-TOF-MS detector in positive and negative ion mode.A standard spectrum library was established by reference standards,and the qualitative analysis was finished by the comparison of the retention time,parent ion and fragment ion accurate molecular mass of each compound in the sample and the library.[Results]The method was specific without interference of blank matrix,and repeatable in sextuplicate.The detection limits of 52 compounds in 5 matrix were 1‒100 mg‧kg^(−1).The method was successfully applied to the analysis of actual samples,and 16 compounds were checked out in 246 samples.[Conclusion]The method is accurate,specific and sensitive,which can be used to combat the illegal adulteration behavior effectively.
作者
孙健
诸艳蓉
胡青
于泓
张静娴
刘贤贤
季申
SUN Jian;ZHU Yanrong;HU Qing;YU Hong;ZHANG Jingxian;LIU Xianxian;JI Shen(NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai Institute for Food and Drug Control,Shanghai 201203,China)
出处
《上海预防医学》
CAS
2022年第6期519-525,共7页
Shanghai Journal of Preventive Medicine
基金
国家自然科学基金(81903800)
上海市自然科学基金(19ZR1448300)
上海市科学技术委员会研发平台专项项目(21DZ2290200)。
关键词
超高效液相色谱-四极杆飞行时间质谱
非法添加
减肥
食品
定性筛查
ultra high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry
illegal adulteration
weight-losing
food
qualitative screening
