摘要
建立了酸水解植物蛋白及酱油中3-氯．1，2-丙二醇（3-MCPD）的固相萃取-气相色谱／质谱测定方法：样品经Aoisa．HBL固相萃取柱萃取，正己烷．乙酸乙酯净化提取，七氟丁酰咪唑衍生，衍生物经气相色谱／负化学电离-质谱（GC／NCI-MS）选择离子模式（SIM）检测，外标法定量。3-MCPD的定量检测限为0．5μg／kg，平均回收率为92．2％～97．4％，相对标准偏差为3．6％～10．9％。该方法检测灵敏度高，定性定量准确。
Solid phase extraction （SPE） and gas chromatographic/negative chemical ionization-mass spectrometric （GC/NCI-MS） method was developed for the determination of 3- monochloropropane-1,2-diol （3-MCPD） in hydrolyzed vegetable proteins （HVP） and soy. The optimized conditions for the extraction and cleanup of 3-MCPD on an Aoisa-HBL column were investigated. The extract with hexane-ethyl acetate was evaporated to nearly dry by N2 at 40 ℃ and derivatization was performed with 1-（heptafluorobutyryl） imidazole at 70 ℃ for 30 min. The mixture was then injected into a gas chromatograph with a DB-5MS capillary column, detected by a mass spectrometer in negative chemical ionization and selected ion monitoring mode （NCI/SIM） and quantified with external standard calibration. The limit of quantitation （LOQ） for 3-MCPD was 0.5 μg/kg. The average recovery was in a range of 92.2% - 97.4% with a rel- ative standard deviation range of 3.6% - 10.9%. The results indicated that the method could be used for the sensitive and accurate determination of 3-MCPD in foods and agriculture products.
出处
《色谱》
CAS
CSCD
北大核心
2006年第5期447-450,共4页
Chinese Journal of Chromatography
基金
国家质量监督检验检疫总局科技计划项目(No.K026-2000)
关键词
气相色谱/质谱法
负化学电离源
选择离子扫描
固相萃取
3-氯-1
2-丙二醇
水解植物蛋白
酱油
gas chromatography/mass spectrometry （GC/MS）
negative chemical ionization（NCI）
selected ion monitoring （SIM）
solid phase extraction （SPE）
3-monochloropropane-I ,2-diol
hydrolyzed vegetable proteins
soy
