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固相萃取-高效液相色谱联用测定食用油中的4种多环芳烃

ISSN号：1003-7969
期刊名称：《中国油脂》
时间：0
分类：TS225[轻工技术与工程—粮食、油脂及植物蛋白工程;轻工技术与工程—食品科学与工程] TS201.6[轻工技术与工程—食品科学;轻工技术与工程—食品科学与工程]
作者机构：[1]武汉大学化学与分子科学学院,生物医学分析化学教育部重点实验室,武汉430072
相关基金：国家自然科学基金（91017013,21005057,91217309）; 中央高校基本科研业务费专项资金（2042014kf 0262）

关键词：食用油, 多环芳烃, 测定, 固相萃取, 高效液相色谱-荧光检测, edible oil, polycyclic aromatic hydrocarbons（PAHs）, determination, solid-phase extraction, high performance liquid chromatography-fluorescence detection

中文摘要：

采用固相萃取与高效液相色谱-荧光检测联用技术,建立了食用油中4种多环芳烃（PAHs）,即（Chr）、苯并（a）蒽（Ba A）、苯并（b）荧蒽（Bb F）和苯并（a）芘（Ba P）的快速分析方法。自制固相萃取小柱,并优化了固相萃取条件。结果表明,食用油样品经异丙醇稀释后可直接进行固相萃取分析。固相萃取优化条件为：BenzoⅡSPE填料1.0 g,洗脱液丙酮8 mL,清洗液异丙醇4 mL,上样液为2 mL 0.2 g/mL的异丙醇稀释油样。4种PAHs在1～50 ng/mL（苯并（b）荧蒽为2～50 ng/mL）质量浓度范围内具有良好的线性关系,相关系数在0.999 2～0.999 8之间,检出限为0.14～0.76ng/g,日内、日间相对标准偏差在2.7%～9.9%之间。对中国计量科学研究院提供的3份橄榄油样品PAHs测定的结果与所给参考值（1号油样Ba P含量）相差10.3%。建立的方法可用于多种食用油中4种PAHs的分析检测,具有耗时短、有机溶剂消耗少、简便快速等优点。

英文摘要：

A rapid method for the determination of four polycyclic aromatic hydrocarbons（ PAHs）（ Chr,Ba A,Bb F and Ba P） in edible oil was developed by solid- phase extraction coupled with high performance liquid chromatography- fluorescence detection（ HPLC- FLD）. The solid- phase extraction column was self- made and the solid- phase extraction conditions were optimized. The results showed that the edible oil sample could be analyzed directly by solid- phase extraction after it was diluted in isopropanol. The optimal solid- phase extraction conditions were obtained as follows： 1. 0 g Benzo ⅡSPE,with 8 mL acetone as desorption solvent,4 mL isopropanol as washing solvent,2 mL 0. 2 g / mL isopropanol diluted oil. The linearity range,correlation coefficient,the limit of detection and relative standard deviation of the proposed method were 1- 50 ng / mL（ 2- 50 ng / mL for Bb F）,0. 999 2- 0. 999 8,0. 14- 0. 76 ng / g and 2. 7%-9. 9%. The relative error between determined value and reference value of Ba P in three kinds of olive oils provided by National Institute of Metrology in China was 10. 3%. The established method had the items of short time,small consumption of organic solvent and simpleness,which was suitable for the determination of four PAHs in edible oils.