液相色谱串联质谱法测定苦丁茶中孔雀石绿残留量

Determination of Malachite Green Residues in Ilex latifolia Thunb.Leaves Tea by LC-MS/MS

应用液相色谱-串联质谱法(LC-MS/MS)测定苦丁茶中孔雀石绿(以孔雀石绿和隐色孔雀石绿之和计)残留量。苦丁茶样品粉碎后复水,用1%乙酸乙腈为提取剂,均质子涡旋1 min,无水硫酸镁和无水乙酸钠除去水,离心后取上清液经净化剂净化后,采用液相色谱-三重四级杆串联质谱仪多反应检测模式(MRM)检测,使用氘代物做内标定量。检测方法的检出限为0.5μg/kg,定量限为1.5μg/kg,线性范围为0.2~10 ng/mL,加标浓度在1.5~15μg/kg时,回收率在80%~100%范围内,相对标准偏差小于10%。实验表明,该方法稳定准确,适用于苦丁茶中孔雀石绿残留量的定性定量测定。

The content of malachite green residues in Ilex latifolia Thunb.leaves tea was determined by LCMS/MS.After the sample of tea was comminuted and rehydrated,1%acetonitrile acetate was used as the solvent,the average proton vortex for 1 min,anhydrous magnesium sulfate and anhydrous sodium acetate were used to remove water.After centrifugation,the supernatant was purified by purification agent,and then detected by liquid chromatography-triple quadrupole tandem mass spectrometer with multi reaction detection mode(MRM).Deuterium was used as internal standard.The detection limit of detection method is 0.5μg/kg,quantitative 1.5μg/kg,linear range is 0.2~10 ng/mL,the average recovery is 80%~100%and the relative standard deviation is less than 10%when the concentration is 1.5~15μg/kg.The results show that the method is stable and suitable for the detection of malachite green residues in Ilex latifolia Thunb.leaves tea.