建立了高效液相色谱-三重四极杆质谱(HPLC-MS/MS)测定面粉中7种荧光增白剂(FWAs)的分析方法.在样品中加入30 mL乙酸乙酯,超声提取10 min,离心后在40℃下氮吹浓缩,用乙腈定容后,上机检测.选用Phenomenex Kinetex C18色谱柱(100 mm×2.1 mm,2.6 μm)分离,以0.1％ (v/v)甲酸-乙腈和水为流动相进行梯度洗脱,采用电喷雾离子(ESI)源,在正离子、多反应监测(MRM)模式下进行扫描,外标法定量.7种荧光增白剂在各自范围内线性关系良好,相关系数均大于0.99,检出限(S/N=3)为0.50 ～2.65 μg/kg,定量限(S/N=10)为1.60～ 8.80μg/kg;在3个添加水平下的平均加标回收率为64.8％ ～ 117.5％,相对标准偏差(n=6)为0.9％ ～ 14.4％.该方法操作简单、回收率高、精密度好,适于面粉中7种荧光增白剂的测定.
A method for the determination of seven fluorescent whitening agents (FWAs) in flour by high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS) was developed.The samples were extracted with ethyl acetate.Then the extracts were centrifuged,concentrated,diluted with acetonitrile and analysed by HPLC-MS/MS.The analysis was carried out on a Phenomenex Kinetex C18 column (100 mm×2.1 mm,2.6 μm) by gradient elution with (A) 0.1％ (v/v) formic acid in acetonitrile and (B) water.Electrospray ionization (ESI) source was operated in the positive mode using multiple reaction monitoring (MRM) scanning mode.The results were quantitated by external standard method.The results indicated that the method had good linear relationships with correlation coefficients (r) not less than 0.99.The limits of detection (LODs) were 0.50-2.65 μg/kg and the limits of quantitation (LOQs) were 1.60-8.80 μg/kg.The average recoveries (n=6) at three spiked levels were in the range of 64.8％-117.5％,and the relative standard deviations (RSDs) were in the range of 0.9％-14.4％.The method has the advantages of simple operation,high recovery and good precision.It is suitable for the simultaneous determination of the seven FWAs in flour.
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