应用高效液相色谱-串联质谱法快速测定水果中的氯吡脲残留量。水果样品经乙腈均质提取,以N-丙基乙二胺、C18和无水硫酸镁作吸附剂净化。所得净化液以C18色谱柱为分离柱,以不同体积比混合的甲醇和5 mmol·L-1乙酸铵溶液为流动相梯度洗脱进行分离,采用电喷雾正离子源多反应监测模式检测。氯吡脲的质量浓度在0.005~0.200 mg·L-1范围内与峰面积呈线性关系,测定下限(10S/N)为1.0 μg·kg-1。在0.01,0.05,0.10 mg·L-1 3个浓度水平进行加标回收试验,回收率在86.4%~106%之间,相对标准偏差(n=6)在3.2%~9.5%之间。

HPLC-MS/MS was applied to the rapid determination of residual amount of forchlorfenuron in fruits. The fruit sample was extracted with acetonitrile by homogeneous stirring and purified with adsorbents of N-propyl-ethylene diamine, C18 and anhydrous magnesium sulfate. The purified sample solution was separated by using C18 column as stationary phase, and mixtures of methanol and 5 mmol·L-1 ammonium acetate solution mixed in different ratios were used as mobile phase in gradient elution. ESI+ as well as multi-reaction monitoring was adopted in MS/MS. Linear relationship between values of peak area and mass concentration of forchlorfenuron was kept in the range of 0.005-0.200 mg·L-1, with lower limit of determination (10S/N) of 10 μg·kg-1. Tests for recovery were made at concentration levels of 0.01, 0.05 and 0.10 mg·L-1 of standard solution, values of recovery found were in the range of 86.4%-106% with RSD′s (n=6) in the range of 3.2%-9.5%.