色谱Issue(3)：256-266,11.DOI:10.3724/SP.J.1123.2014.11001
高效液相色谱-离子阱质谱法快速筛查改善睡眠类保健食品中非法添加的24种镇静催眠药
Fast screening of 24 sedative hypnotics illegally added in improving sleep health foods by high performance liquid chromatography-ion trap mass spectrometry
摘要
Abstract
A fast screening method was established for the simultaneous determination of 24 sedative hypnotics illegally added in improving sleep health foods by high performance liquid chromatography-ion trap mass spectrometry( HPLC-IT MS). The method was based on the son-ication assisted extraction of the improving sleep health food samples using methanol. The ex-tract was then filtrated with 0. 45 μm filter membrane and the filtrate was separated on a Phe-nomenex Luna C18 column with isocratic elution at a flow rate of 0. 3 mL/min. A binary mobile phase was 0. 05%(v/v)formic acid(solvent A)-methanol/acetonitrile(15:25,v/v,solvent B). The electrospray ionization( ESI)source in positive ion mode or negative ion mode was used to scan MS1—MS3 spectra for the 24 sedative hypnotics. The MS2 and MS3 spectra were used for qualitative analysis of samples. The calibration graphs were linear in their concentra-tion ranges with the correlation coefficients( r2 ) more than 0. 999. The limits of detection ( LODs)were 4. 0—446. 6 μg/L. The recoveries for all the drugs in the improving sleep health foods were 88. 6%—110. 3% with the relative standard deviations no more than 9. 8% at three spiked levels. Twenty-seven batches of the improving sleep health foods were tested. Melatonin was found in eighteen batches. The method is fast,specific,sensitive,easy and suitable for fast screening of 24 sedative hypnotics illegally added in improving sleep health foods.关键词
高效液相色谱-离子阱质谱/镇静催眠药品/保健食品/快速筛查Key words
high performance liquid chromatography-ion trap mass spectrometry ( HPLC-IT MS)/sedative hypnotics/health foods/fast screening分类
化学化工引用本文复制引用
芦丽,宫旭,谭力..高效液相色谱-离子阱质谱法快速筛查改善睡眠类保健食品中非法添加的24种镇静催眠药[J].色谱,2015,(3):256-266,11.基金项目
中国食品药品检定研究院项目（2012BAK08B02）． （）
