固相萃取-气相色谱-串联质谱法测定紫菜中扑草净的残留量

Determination of prometryn residues in Pyropia spp. by solid phase extraction-gas chromatography-tandem mass spectrometry

中文关键词:  固相萃取  气相色谱-串联质谱法  扑草净  紫菜

英文关键词:solid phase extraction  gas chromatography-tandem mass spectrometry  prometryn  Pyropia spp

中文摘要:

      目的 建立固相萃取-气相色谱-串联质谱法测定紫菜中扑草净的残留量。方法 样品用乙腈提取, 经活性炭/氨基复合柱(Envi-Carb/NH2)净化, 经Rxi-5MS 石英毛细管色谱柱分离, 采用电子轰击源质谱检测, 选择离子监测(selective ion monitoring, SIM)模式检测, 外标法定量。结果 扑草净在2~1000 μg/L 范围内具有良好的线性关系, 相关系数r2=0.9998。扑草净在5、10、20、50 μg/kg 4 种条件下, 样品加标回收率在95.1%~107.9%, RSD 在5.36%~7.77%(n=6), 方法检出限为1 μg/kg, 定量限为4 μg/kg。结论 该方法操作简单,准确度与精密度较好, 能快速简便地检测紫菜中扑草净的残留量。

英文摘要:

      Objective To establish a method for purification and determination of prometryn residues in Porphyra spp. by solid phase extraction (SPE) columns and gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods The prometryn residues were extracted twice by acetonitrile, purified by Envi-Carb/LC-NH2 column, and analyzed by GC-MS/MS. Rxi-5MS capillary chromatographic column was used for separation, and the selected reaction monitoring with electron impact ionization source was adopted in MS. The data was identified and quantified with external standard method. Results Prometryn had a good linear relationship in the range of 2-1000 μg/L, and the correlation coefficient was 0.9998. When spiked with 5, 10, 25 and 50 μg/kg of prometryn, the recoveries were in the range of 95.1%-107.9%, and the RSD were in the range of 5.36%-7.77% (n=6).The limit of detection was 1 μg/kg, and the limit of quantification was 2 μg/kg. Conclusion The method is simple, accurate and precise, which can quickly and easily detect the prometryn residues in Porphyra spp.