高效液相色谱-串联质谱法测定植物油中吡噻菌胺残留

Determination of penthiopyrad in vegetable oil by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  吡噻菌胺  植物油

英文关键词:high performance liquid chromatography-tandem mass spectrometry  penthiopyrad  vegetable oil

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定植物油中吡噻菌胺的分析方法。方法 称取5.00 g试样于50 mL具塞离心管中, 加入少许氯化钠涡旋1 min, 准确加入10 mL乙腈再涡旋1 min, 超声提取15 min, 4000 r/min离心5 min。取上清液5 mL, 分别加入300 mg十八烷基三甲氧基硅烷粉(C18)和300 mg N-丙基乙二胺粉(primary secondary amine, PSA), 充分涡旋混匀后, 过0.22 μm有机膜后供液相色谱-串联质谱仪测定。以乙腈-0.1%乙酸水为流动相, 经C18柱色谱柱分离后在高效液相色谱-串联质谱多反应监测(multiple reaction monitoring, MRM)模式下分析, 外标法定量。结果 植物油中吡噻菌胺的检出限为2 μg/kg, 定量限为6 μg/kg, 在0.5~200.0 μg/L范围内线性关系较好(r2=0.9967), 在2、4、10 μg/kg 3个浓度水平的加标回收实验下测得, 吡噻菌胺的平均回收率为84.2%~95.3%, 相对标准偏差(relative standard deviations, RSDs)为4.9%~7.8%。结论 该方法操作简单、快速、结果准确, 适用于植物油中吡噻菌胺的分析和检测。

英文摘要:

      Objective To establish a method for the determination of penthiopyrad in vegetable oil by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The 5.00 g of sample was weighed into a 50 mL centrifuge tube with adding a little sodium chloride and vortex for 1 min, then 10 mL acetonitrile was added as extraction solvent with vortex again for 1 min, and extracted for 15 min by ultrasonic. The sample tubes were centrifuged at 4000 r/min for 5 minutes. Then 300 mg octadecyl trimethoxysilane powder (C18) and 300 mg primary secondary amine (PSA) powder were added into 5 mL of supernatant, mixed well by vortex, and determined by HPLC-MS/MS after filtered through a 0.22 μm membrane. Using acetonitrile and 0.1% acetic acid as mobile phase, after separation by C18 column, it was analyzed at the mode of multiple reaction monitoring (MRM) of HPLC-MS/MS and quantified by external standard method. Results The limits of detection and limits of quantitation for the penthiopyrad were 2 μg/kg and 6 μg/kg, respectively. The linear relationships were good in the range of 0.5?200.0 μg/L. Under the standard addition recovery experiment at 3 concentration levels of 2, 4 and 10 μg/kg, the average recoveries of penthiopyrad were 84.2%?95.3%, and relative standard deviations (RSDs) were 4.9%?7.8%. Conclusion This method is simple and fast and the results are accurate, which is suitable for the analysis and determination of penthiopyrad in vegetable oil.