基质分散液-液微萃取结合高效液相色谱-串联质谱法测定商品大米中的8种荧光增白剂

Determination of 8 kinds of fluorescent whitening agents in commercial rice by matrix synchronous dispersive liquid-liquid microextraction combined with high performance liquid chromatography-tandem mass spectrometry

目的 建立基质分散液-液微萃取(matrix synchronous dispersive liquid-liquid microextraction,MS-DLLME)结合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定商品大米中8种荧光增白剂(fluorescent whitening agents,FWAs)的分析方法。方法MS-DLLME通过将基质与水、甲醇和甲苯混合在一个系统中进行,然后通过振荡和离心快速富集和分离目标分析物。结果 8种荧光光谱分析在各自的范围内均获得了良好的线性关系(r>0.99)。加标阴性样品的回收率在76.2%-105.1%之间。相对标准偏差(n=6)在2.1%-9.5%之间。方法检出限为0.01-0.05μg/kg,定量限为0.05-0.20μg/kg。在30份市售大米样品中,检测到2份FWA184阳性样品和1份FWA162阳性样品,证明了该方法的可靠性。结论 该方法具有简便、快速、灵敏和绿色的特点,适用于大米中8种荧光增白剂的测定。

Objective To establish a method for the determination of 8 kinds of fluorescent whitening agents(FWAs) by matrix synchronous dispersive liquid-liquid microextraction(MS-DLLME) combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) for the analysis of in commercial rice. Methods MS-DLLME was performed by mixing matrix with water, methanol and toluene in one system, then target analytes were rapidly enriched and separated through simple shaking and centrifugation. Results Eight kinds of fluorescent whitening agents obtained good linear relationship in their respective ranges(r>0.99). The recoveries of spiked negative samples ranged from 76.2% to 105.1%. The relative standard deviations(n=6) were between 2.1% and 9.5%. The limits of detection of the method were 0.01-0.05 μg/kg, the limits of quantitative were 0.05-0.20 μg/kg. Two FWA184 positive samples and one FWA162 positive sample were detected in 30 commercial rice samples, which proved the reliability of the method. Conclusion This method is simple, rapid, accurate and green, and is suitable for the determination of 8 kinds of fluorescent whitening agents in rice.