分析测试学报2018，Vol.37Issue(4)：434-439,6.DOI:10.3969/j.issn.1004-4957.2018.04.008
固相萃取/液相色谱-串联质谱法测定麦卢卡蜂蜜特征化合物
Determination of Characteristic Compounds in Manuka Honey by Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction
摘要
Abstract
A solid phase extraction/liquid chromatography-tandem mass spectrometric (SPE/LC-MS/MS) method was established for the simultaneous determination of 2'-methoxyacetophenone (2'-MAP),2-methoxybenzoic acid (2-MBA),3-phenyllactic acid (3-PA) and 4-hydroxyphenyllactate (4-HPA).The honey sample was dissolved in 1％ formic acid solution,then purified with HLB SPE.The separation of the analytes was performed on a Thermo Hypersil Gold C1s (50 mm × 2.1 mm,1.9 μm) column with 0.1％ formic acid solution and acetonitrile containing 0.1％ formic acid as mobile phases by gradient elution.The four compounds were detected simultaneously in electrospray negative and positive ionization modes under multiple reaction monitoring(MRM) mode.The results showed that the calibration curves were linear in the range of 0.01-1.0 mg/L for 2'-MAP,2-MBA and 4-HPA,and 0.1-10.0 mg/L for 3-PA with correlation coefficients(r2) higher than 0.99.The limits of detection(LODs) and quantitation(LOQs) were in the ranges of 0.1-1.0 mg/kg and O.5-5.0 mg/kg,respectively.The average spiked recoveries for honey samples ranged from 79.4％ to 98.3％ with relative standard deviations (n =6) of 3.2％-8.7％.This method was used to validate 114 hive honey samples from 12 varieties collected in different locations in New Zealand and 50 commercial honey samples from four different countries.With the charateristics of sensitivity,accuracy and rapidness,the method could provid a reference for the identification of monoflower,multiflower and non-manuka honey.关键词
固相萃取/液相色谱-串联质谱(SPE/LC-MS/MS)/特征化合物/麦卢卡蜂蜜Key words
solid phase extraction/liquid chromatography-tandem mass spectrometry (SPE/LC-MS/MS)/characteristic compound/manuka honey分类
化学化工引用本文复制引用
郭思言,邓晓军,伊雄海,杨功俊,王雪婷,丁涛,吴斌,张峰,冯峰,刘芸,柳菡,张晓燕,陈磊..固相萃取/液相色谱-串联质谱法测定麦卢卡蜂蜜特征化合物[J].分析测试学报,2018,37(4):434-439,6.基金项目
国家重点研发计划(2017YFF0211000) （2017YFF0211000）
国家质检总局科技计划项目(2016IK135) （2016IK135）
