摘要
建立超高效液相色谱-串联质谱法同时测定食品中4种木酚素(包括亚麻木酚素、芝麻素、芝麻林素和芝麻酚)的分析方法。试样采用含1 mol/L氢氧化钠(NaOH)的70%乙醇水溶液提取,盐酸调节pH至4~4.5,用70%乙醇水定容。以甲醇和0.1%甲酸水为流动相梯度洗脱,经C18色谱柱分离;采用电喷雾电离源,正离子模式(ESI+),选择反应监测模式扫描(SRM),外标法定量。结果表明:4种木酚素在0.040~10μg/mL浓度范围内线性关系良好,相关系数R在0.9995~0.9999之间;相对标准偏差(RSD)为1.0%~3.1%;在50~2.00×103 mg/kg的加标浓度范围内,回收率为95.0%~101%。亚麻木酚素、芝麻酚、芝麻素、芝麻林素的检出限分别为0.1,0.1,0.03和0.1 mg/kg。该方法分离效果好,灵敏度和准确度高,简单快速,适用范围广。
A method for determination of 4 lignans(including seco-isolariciresinol diglucoside,sesamol,sesamin and sesamolin)by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed.The sample was extracted with 70%ethanol aqueous solution containing 1 mol/L sodium hydroxide(NaOH),the pH was adjusted to 4-4.5 with hydrochloric acid,and the volume was adjusted with 70%ethanol water.Four analytes were separated on a C18 column by gradient elution with a mobile phase consisting of 0.1%formic acid/water and methanol.The detection was performed using UPLC-ESI-MS/MS detector with selective reaction monitoring(SRM)in positive mode.External standard method was used for qualification.The results show that this method had a good linearity in the concentration range of 0.040-10μg/mL,the correlation coefficient was 0.9995-0.9999,RSD was 1.0%-3.1%,and the recoveries in the spiked levels of 50-2.00×103 mg/kg were in the range of 95.0%-101%.The limits of detection of SDG,sesamol,sesamin and sesamolin in food were 0.1,0.1,0.03 and 0.1 mg/kg,respectively.The method had good separation effect,high sensitivity,high accuracy,simpleness,speediness,and wide application range.
作者
肖伟敏
王奇
董珊
苏佳婷
彭祖茂
张协光
XIAO Weimin;WANG Qi;DONG Shan;SU Jiating;PENG Zumao;ZHANG Xieguang(Shenzhen Academy of Metrology and Quality Inspection,National Nutrition Food Testing Center(Guangdong),Shenzhen 518109)
出处
《食品工业》
CAS
北大核心
2020年第4期294-298,共5页
The Food Industry
基金
深圳市标准计划(2018-WB24)
深圳市计量质量检测研究院科技项目(2017-YA34)。
