液液萃取-高效液相色谱法同时测定植物油中的毒黄素、路霉素和热诚菌素  

Determination of Toxoflavin,Reumycin and Fervenulin in Vegetable Oil by Liquid-Liquid Extraction-High Performance Liquid Chromatography

作　　者：王朝霞 尹芳平 汪辉 周鹏 邓楠 曾辉 胡宇格 Wang Zhaoxia;Yin Fangping;Wang Hui;Zhou Peng;Deng Nan;Zeng Hui;Hu Yuge(Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410111;Changsha Institute for Food and Drug Control,National Centre of Quality Supervision and Testing of Alcoholic Products,Changsha 410000)

机构地区：[1]食品安全监测与预警湖南省重点实验室,长沙410111 [2]长沙市食品药品检验所,国家酒类产品质量监督检验中心,长沙410000

出　　处：《中国粮油学报》2022年第1期175-181,共7页Journal of the Chinese Cereals and Oils Association

基　　金：食品安全监测与预警湖南省重点实验室开放基金项目(2020KFJJ07)。

摘　　要：通过优化样品前处理方法,建立了高效液相色谱法测定植物油中的毒黄素、路霉素和热诚菌素的含量。样品采用甲醇液液萃取、氮吹浓缩,经高效液相色谱仪分析检测,外标法定量。采用Ultimate AQ-C18(4.6 mm×250 cm,5μm)色谱柱分离,流速为1.0 mL/min,流动相为0.1%甲酸-甲醇(90∶10),检测波长为240 nm。在优化条件下,3种目标化合物在0~40.0μg/mL线性范围内线性良好;毒黄素、路霉素和热诚菌素的方法检出限(S/N≥3)均为0.8 mg/kg,方法定量限(S/N≥10)均为3.2 mg/kg;在3.2~32 mg/kg的添加范围内,毒黄素的回收率为98.93%~109.44%,方法精密度(RSD,n=6)小于6.81%;路霉素的回收率为102.85%~109.77%,方法精密度(RSD,n=6)小于4.26%;热诚菌素的回收率为95.26%~101.54%,方法精密度(RSD,n=6)小于4.30%,所测11种食用植物油样品中3种目标化合物均未检出。本方法简便、准确、精密度和回收率好,可用于食用植物油中毒黄素、路霉素和热诚菌素的检测。A high performance liquid chromatography(HPLC)method was established for the determination of toxoflavin,reumycin and fervenulin in vegetable oil by optimizing the sample pretreatment method.The samples were extracted by methanol,concentrated by nitrogen blowing,analyzed by HPLC,and quantified by external standard method.Ultimate AQ-C18(4.6 mm×250 cm,5μm)chromatographic column was used for separation.The flow rate was 1.0 mL/min,and the mobile phase was 0.1%formic methanol(90∶10).The detection wavelength was 240 nm.Under optimal conditions,the three target compounds showed good linearity in the linear range of 0~40.0μg/mL.The detection limit of toxoflavin,reumycin and fervenulin were 0.8 mg/kg,and the quantitative limit of methods was 3.2 mg/kg.In the range of 3.2~32 mg/kg,the recovery of toxoflavin(n=6)was 98.93%~109.44%,the method precision(RSD)was less than 6.81%,the recovery of reumycin(n=6)was 102.85%~109.77%,the method precision(RSD)was less than 4.26%,and the recovery(n=6)of fervenulin was 95.26%~101.54%,the method precision(RSD)was less than 4.30%.None of the three target compounds were detected in the 11 vegetable oil samples tested.This method was simple,accurate precision and had a good recovery rate.It can be used for the detection of vegetable oil toxoflavin,Reumycin and fervenulin.

关 键 词：液液萃取 高效液相色谱 植物油 毒黄素 路霉素 热诚菌素 

分 类 号：TS227[轻工技术与工程—粮食、油脂及植物蛋白工程]