提出了固相萃取-高效液相色谱-串联质谱法测定香蕉中咪鲜胺及2,4,6-三氯苯酚残留量的方法。香蕉样品经乙酸-乙腈(2+98)混合液提取,用基质分散固相萃取净化。以Agilent Eclipse AAA色谱柱为分离柱对所得净化液进行分离,以不同体积比的水和乙腈混合液为流动相进行梯度洗脱,采用电喷雾正、负离子源多反应监测模式检测。咪鲜胺和2,4,6-三氯苯酚的线性范围分别为0.05~100 mg·L-1和2.5~200 mg·L-1,检出限(3S/N)分别为0.02,1.5 μg·kg-1。以空白样品为基体进行加标回收试验,测得咪鲜胺和2,4,6-三氯苯酚的回收率分别在90.3%~106%和85.5%~101%之间,相对标准偏差(n=6)分别在3.3%~8.5%和3.6%~9.6%之间。

A method of HPLC-MS/MS for determination of residual amounts of prochloraz and 2,4,6-trichlorophenol in banana with solid phase extraction was proposed. The banana sample was extracted with a mixture of acetic acid and acetonitrile (2+98) and purified by matrix dispersion solid phase extraction. The purified sample solution was separated by using Agilent Eclipse AAA column as stationary phase, and mixtures of acetonitrile and water in different ratios as mobile phase in gradient elution. ESI+, ESI- and multi-reaction monitoring were adopted in MS/MS. Linearity range was found between 0.05-100 mg·L-1 for prochloraz, and between 2.5-200 mg·L-1 for 2,4,6-trichlorophenol, with detection limits (3S/N) of 0.02 μg·kg-1 for prochloraz and 1.5 μg·kg-1 for 2,4,6-trichlorophenol. Using blank samples as matrixes, test for recovery was made by standard addition method, giving recovery of prochloraz and 2,4,6-trichlorophenol in the ranges of 90.3%-106% and 85.5%-101% respectively, with RSD′s (n=6) in the ranges of 3.3%-8.5% and 3.6%-9.6% respectively.