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

中文关键词:  高效液相色谱-质谱联用法  违禁色素  豆制品  残留分析

英文关键词:high-performance liquid chromatography-mass spectrometry  prohibited pigment  bean products  residue analysis

中文摘要:

      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-C18色谱柱(50 mm×2.1 mm, 3.1 μm)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(r2)均大于0.999, 加标水平为2.0 μg/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2.0 μg/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。

英文摘要:

      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-C18 column(50 mm×2.1 mm, 3.1 μm)and separated with gradient elution, with the mobile phases of methanol and 0.1% 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 (r2) were more than 0.999. When the standard was 2 μg/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.