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高效液相色谱-串联质谱法快速测定水果中氯吡脲残留量
Rapid Determination of Residual Amount of Forchlorfenuron in Fruits by HPLC-MS/MS
【摘要】 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5mmol·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0.005~0.200mg·L-1范围内与峰面积呈线性关系,测定下限(10S/N)为1.0μg·kg-1。在0.01,0.05,0.10mg·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。
【Abstract】 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 Npropyl-ethylene diamine,C18and anhydrous magnesium sulfate.The purified sample solution was separated by using C18column as stationary phase,and mixtures of methanol and 5mmol·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 10μg·kg-1.Tests for recovery were made at concentration levels of 0.01,0.05and 0.10mg·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%.
- 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis(Part B:Chemical Analysis) , 编辑部邮箱 ,2014年02期
- 【分类号】O657.63;TS255.7
- 【被引频次】15
- 【下载频次】184