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(C_(18))和300 mg N-丙基乙二胺粉(primary secondary amine, PSA),充分涡旋混匀后,过0.22μm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C_(18)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2μg/kg,定量限为6μg/kg,在0.5~200.0μg/L范围内线性关系较好(r^(2)=0.9967),在2、4、10μg/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。
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(C_(18)) 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 C_(18) 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.
作者
陆静
朱绍华
付善良
申甜甜
陈练
成婧
LU Jing;ZHU Shao-Hua;FU Shan-Liang;SHEN Tian-Tian;CHEN Lian;CHENG Jing(Hunan Key Laboratory of Food Safety Science&Technology,Technology Center of Changsha Customs,Changsha 410004,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第18期7261-7266,共6页
Journal of Food Safety and Quality
基金
海关总署科技计划项目(2021HK202)
国家质量基础共性技术研究与应用项目(2017YFF0211001)。
关键词
高效液相色谱-串联质谱法
吡噻菌胺
植物油
high performance liquid chromatography-tandem mass spectrometry
penthiopyrad
vegetable oil
