超高效液相色谱-质谱法测定养殖水体孔雀石绿

Determination of malachite green in aquaculture water by ultra performance liquid chromatography-mass spectrometry

为快速、准确监测水产养殖环境水体中孔雀石绿含量,建立了一种超高效液相色谱-串联质谱法（UPLCMS/MS）测定水产养殖水体中孔雀石绿及隐色孔雀石绿的方法.水样经甲酸酸化预处理后,采用多壁碳纳米管固相萃取柱富集和净化目标物,超高效液相色谱分离,三重四级杆质谱检测,氘代同位素内标定量.在优化条件下,孔雀石绿和隐色孔雀石绿在0.02~10.0μg·L-1浓度范围内均满足线性关系,相关系数R2〉0.998,方法检出限、定量限分别为0.000 3和0.001μg·L-1.在0.005~0.100μg·L-1添加水平下,淡水中孔雀石绿加标回收率为98.7%~107.8%,隐色孔雀石绿加标回收率为95.3%~112.6%,海水中孔雀石绿加标回收率为89.5%~92.7%,隐色孔雀石绿加标回收率为94.2%~101.4%,测定相对标准偏差均在7.4%以内.结果表明,所建立的超高效液相色谱-质谱法简单快速、前处理成本低、灵敏度高、重现性好、回收率高,适合于养殖水体中孔雀石绿的测定.

A simple, rapid and cheap approach for determination of malachite green（MG） and leucomalachite green （LMG） in aquaculture water using ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/ MS） has been descrihed. The samples were pretreated with formic acid, then enriched and purified by multi-wall carbon nanotube solid phase extraction. Chromatographic separation was achieved by UPLC and the detection was performed by triple quadrupole mass spectrometry using deuterated isotope internal standard. Under the optimized conditions, the analytes were in good linearity in the range of 0.02- 10.0 μg · L-1 and the correlation coefficients were above 0. 998. The limit of detection and limit of quantity were 0. 000 3 and 0. 001 μg · L-1, respectively. Spiked at levels of 0. 005-0. 100 μg · L-1, the recovery rates of MG, LMG were 98.7%-107.8% and 95.3% 112.6% for freshwater, andMG89.5%-92.7%0, LMG94.2%-101.4% for seawater. The relative standard deviations were all within 7.4%0. It is concluded that this method can be successfully applied for the determination of malachite green in aquaculture water with good reproducibility and high recovery rate.