液相色谱-同位素稀释质谱法检测食用油中辣椒碱类化合物  

Determination of Capsaicinoids in Edible Oil by Liquid Chromatography-isotope Dilution Mass Spectrometry

作　　者：国振[1] 李秀琴[1] 高方园[1,2] 张庆合[1] 李红梅[1] 

机构地区：[1]中国计量科学研究院化学计量与分析科学研究所,北京100029 [2]华东理工大学化学与分子工程学院,上海200237

出　　处：《化学试剂》2016年第6期491-495,共5页Chemical Reagents

基　　金：国家质量监督检验检疫总局公益性行业科研专项项目(2012104010-5);国家重大科学仪器设备开发专项项目(2012YQ09016703);首都食品安全科技创优培育专项项目(Z141100002614009)

摘　　要：建立了食用油中辣椒碱类化合物（包括辣椒素、二氢辣椒素、降二氢辣椒素和合成辣椒素）的液相色谱-同位素稀释质谱准确测定方法。样品中的辣椒碱类化合物用碱液提取后,进行自动固相萃取富集净化、同位素稀释质谱法准确定量。4种化合物在两个浓度水平的平均加标回收率为96.2%-105%,相对标准偏差为0.5%-3.8%（n=6）,方法检出限均为0.015μg/kg。采用该方法分别对食用油样品和＂地沟油＂样品中的辣椒碱含量进行检测。结果表明,大多数食用植物油中未检测出辣椒碱,花生油中辣椒碱本底含量在0-1.8μg/kg范围内,多数地沟油中辣椒碱含量〉600μg/kg,以此可实现正常食用油和地沟油的有效区分,并作为鉴别地沟油的重要手段之一。A method was developed on determination of capsaicinoids（capsaicin,dihydrocapsaicin,nordihydrocapsaicin and n-vanillylnonanamide） in edible oil by liquid chromatography-isotope dilution mass spectrometry（LC-IDMS）.The sample was firstly extracted with sodium hydroxide solution,then the extract was cleaned-up by auto solid phase extraction（SPE） before the LCIDMS analysis.The limit of detection（LOD,S/N〉 3） for capsaicinoids was 0.015 μg/kg,and the recoveries of the 4 kinds of capsaicinoids in edible oil samples were 96.2% - 105% with the RSDs ranged 0.5% - 3.8%（n = 6）.Edible oils and illegal edible oils were both analyzed using this method,and significant differences were observed.The results showed that there were no capsaicinoids in most kinds of edible oils.Peanut oil contained little capsaicinoids ranged 0 - 1.8 μg/kg which may be come from peanut.The content of capsaicinoids was above 600 μg/kg in most illegal cooking oils.This method can be used as one of identification methods on illegal cooking oil.

关 键 词：同位素稀释质谱法 辣椒碱 食用油 地沟油 

分 类 号：O658[理学—分析化学]