超高效液相色谱-串联质谱法检测食用菌中 荧光增白剂

Determination of fluorescent whitening agents in edible mushrooms by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  荧光增白剂  超高效液相色谱-串联质谱法  固相萃取  食用菌

英文关键词:fluorescent whitening agents  ultra performance liquid chromatography-tandem mass spectrometry  solid phase extraction  edible mushrooms

中文摘要:

      目的 建立新鲜食用菌中荧光增白剂85(fluorescent brightener VBL, VBL)、荧光增白剂71(fluorescent brightener CXT, CXT)和荧光增白剂113(blankophor BA, BA)的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS, )定量检测方法。方法 采用60%甲醇-水溶液, 75 ℃水浴振荡提取试样中的荧光增白剂, 经弱阴离子交换固相萃取柱净化, 采用UPLC-MS/MS在负离子模式下检测, 内标法定量。结果 该方法在0.0100~0.500 mg/L范围内有良好的线性关系, 相关系数r2＞0.990, 在空白新鲜食用菌基质中, 不同添加水平下方法的平均回收率范围为80.0%~101%, 相对标准偏差为3.4%~11.9%; 测定低限为0.100 mg/kg。结论 此方法灵敏度高、准确、重现性好, 适用于新鲜食用菌中荧光增白剂85、荧光增白剂71和荧光增白剂113的检测。

英文摘要:

      Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry method for the determination of three fluorescent whitening agents (fluorescent brightener VBL, fluorescent brightener CXT and blankophor BA) in edible mushrooms. Methods The residues of fluorescent whitening agents in the test samples were extracted with 60% methanol water solution by a 75 ℃ shaking water bath. After being cleaned up with weak anion exchange solid-phase extraction column, the residues were detected by ultra performance liquid chromatography-tandem mass spectrometry under multiple reactions monitoring (MRM) mode via negative-ion mode and quantified by an internal standard method. Results The method showed a good linearity over the range of 0.0100~0.500 mg/L for three fluorescent whitening agents with r2>0.990. The average recoveries were 80.0%~101% at three spiked levels in edible mushrooms and the relative standard deviations were 3.4%~11.9%. The limit of quantitation was 0.100 mg/kg. Conclusion This method was highly sensitive, accurate and reproducible, and it could be suitable for the detection of three fluorescent whitening agents VBL, CXT and BA in edible mushrooms.