QuEChERS-超高效液相色谱-串联质谱法快速测定豆制品中二甲基黄和碱性嫩黄O的含量
目的 建立QuEChERS结合超高效液相色谱-串联质谱法(QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry, QuEChERS-UPLC-MS/MS)快速测定豆制品中二甲基黄和碱性嫩黄O的含量。方法 豆制品经20 mL乙腈-水(1:1, V:V)浸泡, 采用QuEChERS方法进行萃取、净化, 经Shim-pack XR-ODS Ⅲ色谱柱分离, 正离子扫描, 多反应监测模式进行质谱分析, 外标法定量。结果 二甲基黄在添加水平为0.5、1和10 μg/kg时, 方法回收率为81.6%~97.2%; 碱性嫩黄O在添加水平为6、10和50 μg/kg时, 方法回收率为89.1%~100.7%; 二甲基黄和碱性嫩黄O的相对标准偏差均小于12%(n=6); 二甲基黄和碱性嫩黄O的检出限分别为0.5、2 μg/kg; 定量限分别为1.5、6 μg/kg。结论 该方法操作简便、快速准确, 适用于豆制品中二甲基黄、碱性嫩黄O的快速筛查和定量分析。
Objective To establish a method for simultaneous determination of dimethyl yellow and auramine O in bean products by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (QuEChERS- UPLC-MS/MS). Methods The bean products were soaked by 20 mL acetonitrile–water (1:1, V:V), extracted and purified by QuEChERS method, separated by Shim-pack XR-ODS Ⅲ column, and then determined by mass spectrometry with positive electrospray ionization and multiple reaction monitoring (MRM) mode. External standard method was used for quantification. Results The recoveries of dimethyl yellow were 81.6%~97.2% when spiked at 0.5, 1 and 10 μg/kg, and the recoveries of auramine O were 89.1%~100.7% when spiked at 6, 10 and 50 μg/kg. The relative standard deviations of the method were less than 12% (n=6). The limits of detection of dimethyl yellow and auramine O were 0.5 and 2 μg/kg, respectively. The limits of quantitation were 1.5 and 6 μg/kg, respectively. Conclusion This method is simple, accurate, and sensitive, which can be used for rapid screening and quantitative analysis of dimethyl yellow and auramine O in bean products.
标题：QuEChERS-超高效液相色谱-串联质谱法快速测定豆制品中二甲基黄和碱性嫩黄O的含量
英文标题：Rapid determination of dimethyl yellow and auramine O in bean products by QuEChERS method combined with ultra performance liquid chromatography-tandem mass spectrometry
作者：
李锦清 广东产品质量监督检验研究院
綦艳 广东产品质量监督检验研究院
廖桂福 广东产品质量监督检验研究院
陈满英 广东产品质量监督检验研究院
中文关键词:QuEChERS,超高效液相色谱-串联质谱法,二甲基黄,碱性嫩黄O,豆制品,
英文关键词:QuEChERS,ultra performance liquid chromatography-tandem mass spectrometry,dimethyl yellow,auramine O,bean products,
发表日期：2016-06-18
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