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作 者:周娜[1,2] 骆和东[2] 李呐[1,2] 李耀群[1]
机构地区:[1]厦门大学化学化工学院化学系与现代分析科学重点实验室,福建厦门361005 [2]厦门市疾病预防控制中心,福建厦门361021
出 处:《光谱学与光谱分析》2014年第3期787-790,共4页Spectroscopy and Spectral Analysis
基 金:国家自然科学基金项目(21127005;20975084);福建省科技重点项目(2009Y0046)资助
摘 要:微波具有萃取效率高、加热均匀、节省时间等特点,而恒能量同步荧光法应用于多环芳烃的检测可提高选择性,导数技术又能放大窄带灵敏度,抑制宽带,改善分辨能力。本文结合恒能量同步荧光扫描技术与导数技术,采用家用微波炉,建立了食品中苯并(α)芘(BaP )的微波辅助萃取-二阶导数恒能量同步荧光法。探讨了影响微波萃取效率的主要因素,如萃取溶剂的类型及使用量、微波萃取时间及冷却时间、微波辐射功率等,并与超声萃取做了比较。对低脂肪样品直接用混合溶剂微波萃取即可进行光谱扫描检测食品中的BaP;对高脂肪样品将皂化和微波辅助萃取这两步操作同时进行,简化操作步骤,缩短样品的前处理时间,使样品的整个分析过程可在1h内完成。该方法操作简单、快速、费用低廉,已应用于实际样检测,低脂肪样品的加标回收率为90.0%~105.0%,高脂肪样品的为83.3%~94.6%,方法重现性好,结果令人满意。Coupling derivative technique and constant-energy synchronous fluorescence scanning technique ,a method of determi-ning benzo [α]pyrene in foods by second derivative constant-energy synchronous spectrofluorimetry after microwave-assisted treatment of samples was established using domestic microwave oven .The main factors of influencing the efficiency of microwave extraction were discussed ,including the extraction solvent types and amounts ,the microwave extraction time ,microwave radia-tion power and cooling time .And the comparison with ultrasonic extraction was made .Low-fat food samples ,which were just microwave-extracted with mixed-solvents ,could be analyzed immediately by the spectrofluorimetric technique .For high-fat food samples ,microwave-assisted saponification and extraction were made at the same time ,thus simplifying operation steps and re-ducing sample analysis time .So the whole sample analysis process could be completed within one hour .This method was simple , rapid and inexpensive .In consequence ,it was applied to determine benzo (α)pyrene in food with good reproducibility and the re-coveries of benzo (α)pyrene ranged from 90.0% to 105.0% for the low fat samples and 83.3% to 94.6% for high-fat samples .
关 键 词:食品 微波萃取 苯并(α)芘 二阶导数-恒能量同步荧光法
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