高效液相色谱-质谱联用技术测定豆制品中7种违禁色素的残留

Determination of 7 kinds of prohibited pigment residues in bean products by high-performance liquid chromatography-mass spectrometry

目的建立高效液相色谱-串联四极杆质谱法(high-performance liquid chromatography-mass spectrometry,HPLC-MS/MS)测定豆制品中二甲基黄、二乙基黄、罗丹明B、碱性橙2、碱性橙21、碱性橙22和碱性嫩黄7种违禁色素残留量的分析方法。方法豆制品经水溶解后,再以乙腈提取7种违禁色素,采用甲醇和0,1%甲酸水溶液作为流动相进行梯度洗脱,流速为0.3 mL/min,经Agilent ZORBAX SB-C_(18)色谱柱(50mm×2.1 mm,3.1μm)进行分离,电喷雾电离源(ESI),正离子模式,多反应监测模式(MRM)对违禁色素的定性离子和定量离子进行监测。结果本方法的线性范围为0~10.0 ng/mL,相关系数(r^2)均大于0.999,加标水平为2.0μg/kg时,回收率范围是80.5%~104.3%,相对标准偏差(n=6)为2.88%~7.63%,检出限为2.0μg/kg。结论该方法前处理简单,分析时间短,适用于对豆制品中7种违禁色素残留的同时检测。

Objective To establish a method for the determination of 7 kinds of prohibited pigments,including dimethyl yellow,rhodamine B,basic ora2,basic ora 21,basic ora 22 and auramine in bean products by high performance liquid chromatography-mass spectrometry（HPLC-MS/MS）.Methods Bean products was dissolved by water,and extracted by acetonitrile.The samples were load onto an Agilent ZORBAX SB-C_（18）column（50 mm×2.1 mm,3.1 μm）and separated with gradient elution,with the mobile phases of methanol and0.1%formic acid,and the flow rate at 0.3 mL/min.The electrospray was operated in the positive mode and the samples were monitored in the multiple reaction monitoring（MRM） mode.Results The linear ranges of the method were 0~10.0 ng/mL,and correlation coefficients（r^2） were more than 0.999.When the standard was 2μg/kg,the recoveries were 80.5%~104.3%.The RSD（n=6） was 2.88%~7.63%,and the LOD was 2 μg/kg.Conclusion This method is simple and rapid,and is suitable for the detection of 7 kinds of prohibited pigment residues in bean products.