超高效液相色谱-串联质谱法测定减肥保健食品中10种减肥类化合物的含量  

UHPLC-MS/MS Determination of 10 Weight Loss Compounds in Slimming Health Foods

作　　者：熊岑[1,2] 林叶婧 李卫岗[3] 张悦[1] 李意[1] 柏文良[1] 

机构地区：[1]深圳市计量质量检测研究院,深圳518000 [2]广东石油化工学院环境与生物工程学院,茂名525000 [3]珠海出入境检验检疫局技术中心,珠海519000

出　　处：《理化检验（化学分册）》2017年第7期780-786,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：深圳市计量质量检测研究院科研项目(2015-YN41);珠海出入境检验检疫局科技项目(ZH2013-6)

摘　　要：样品(0.500 0g)经甲醇25 mL超声提取20 min后,提取液用甲醇稀释至50 mL,经0.22μm滤膜过滤后进行色谱分离。以Thermo Hypersil Gold色谱柱为固定相,以不同体积比的乙腈和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾离子源正负离子切换模式和多反应监测模式。10种化合物的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3S/N)在0.01~1.00μg·g^(-1)之间。按标准加入法进行回收试验,回收率在72.1%~117%之间,测定值的相对标准偏差(n=5)在0.70%~6.2%之间。The sample （0. 500 0 g） was extracted ultrasonically for 20 min with 25 mL of methanol, and the extract was diluted to 50 mL with methanol, and filtered through microporous membrane of 0.22 μm. The solution was then separated by UHPLC using Thermo Hypersil Gold column as stationary phase and a mixture of acetonitrile and 0.1% （φ） formic acid solution in various ratios as mobile phase in gradient elution. ESI with switching mode of positive ions and negative ions and MRM were adopted in MS. Linear relationships between values of peak area and mass concentration of 10 compounds were found in definite ranges, with detection limits （3S/N） in the range of 0. 01 1.00 μg · g^-1. Test for recovery was made by standard addition method, giving results in the range of 72.1%-117%, with RSDs （n=5） ranged from 0. 70% to 6.2%.

关 键 词：超高效液相色谱-串联质谱法 减肥类化合物 减肥类保健食品 

分 类 号：O652.61[理学—分析化学]