QuEChERS-UPLC-MS/MS法测定龟甲中孔雀石绿和隐性孔雀石绿残留量

Determination of residual malachite green and leucomalachite green in tortoise shell by QuEChERS-UPLC-MS/MS

目的:建立超高效液相色谱-串联三重四极杆质谱法快速测定龟甲中孔雀石绿和隐性孔雀石绿残留量的检测方法。方法:样品采用5%甲酸乙腈溶液提取,用二异氰酸酯多元醇共聚物(EMR)净化,采用C_(18)色谱柱分离,以5 mmol·L^(-1)醋酸铵溶液和乙腈梯度洗脱,采用选择离子监测(Target MS/MS)模式检测。结果:孔雀石绿在0. 096～2. 4μg·L^(-1)范围内线性良好(r=0. 998 9),三个浓度加标回收率为90. 8%～103. 3%(n=9);隐性孔雀石绿在0. 087～2. 18μg·L^(-1)范围内线性良好(r=0. 999 4),三个浓度加标回收率为67. 1%～83. 8%(n=9),多批次样品中检测出孔雀石绿和隐性孔雀石绿。结论:本方法可以用于快速测定龟甲中孔雀石绿和隐性孔雀石绿残留量。

Objective： To establish a UPLC-MS/MS method for rapid determination of the residual malachite green and leucomalachite green in tortoise shell. Methods： The samples were extracted with 5% formic acid acetonitrile solution, purified by diisocyanate polyol copolymer （EMR）, separated by C18 column, eluted in the gradient proce- dure of 5 mmol·L^-1 ammonium acetate solution and acetonitrile, then detected by selective ion monitoring （Target MS/MS） mode. Results： The linear range fell into 0. 096 -2. 4μg·L^-1 （r =0. 998 9）, and the spiked recoveries of three concentration levels were 90. 8% - 103.3% （ n = 9 ） for malachite green. The linear range fell into 0.087-2. 18 μg·L^-1 （r =0.999 4）, and the spiked recoveries of three concentration levels were 67.1% - 83.8% （n = 9） for leucomalachite green. Malachite green and leucomalachit green were be detected in the multiple batches of samples. Conclusion： This method can be used for rapid determination of residual malachite green and leucomalachite green in tortoise shell.