提出了高效液相色谱-四极杆串联线性离子阱质谱法测定水产及饲料中的孔雀石绿、结晶紫及其代谢物(隐色孔雀石绿、隐色结晶紫)的方法。样品经乙腈提取,Agilent XDB C18色谱柱分离,四极杆串联线性离子阱质谱进行检测。以氘代孔雀石绿、氘代隐色孔雀石绿、氘代结晶紫、氘代隐色结晶紫为内标物。4种化合物的线性范围均为0.05~5.0 μg·L-1,检出限(3S/N)均为0.5 μg·kg-1。以空白样品为基体做加标回收试验,计算得4种化合物的回收率在93.3%~120%之间,相对标准偏差(n=6)在1.4%~18%之间。另外,还采用数据相关采集模式结合增强离子扫描模式对4种化合物进行定性分析,可对试样中4种化合物在定量同时进行定性确证。

A method of HPLC-q/LIT-MS for the determination of malachite green, crystal violet and their metabolites (leucomalachite green, leucocrystal violet) were proposed. The sample was extracted with acetonitrile and separated on Agilent XDB C18 chromatographic column and determined by q/LTQ MS. The malachite green D5, crystal violet D6, leucomalachite green D6, and leucocrystal violet D6 were used as internal standards. Linearity ranges of the 4 compounds were found same between 0.05-5.0 μg·L-1 with detection limits (3S/N) of 0.5 μg·kg-1. Using blank samples as matrixes, test for recovery was made by standard addition method, giving recovery of the 4 compounds in the range of 93.3%-120% with RSD′s (n=6) in the range of 1.4%-18%. Furthermore, qualitative analysis for the 4 compounds was performed by applying the modes of information dependent acquisition and enhanced product ion scanning, thus attaining both identification and determination of the 4 compounds.