Imai Koichi, Onoue Keiko, Ishii Rie, Takano Mariko, Nemoto Satoru, Teshima Reiko
Saitama Prefectural Institute of Public Health.
Shokuhin Eiseigaku Zasshi. 2015;56(5):205-10. doi: 10.3358/shokueishi.56.205.
A method for the determination of ipfencarbazone in agricultural products, livestock products and seafood by LC-MS/MS was developed. Agricultural samples were extracted with acetone. An aliquot of crude extract was partitioned with n-hexane and sat. sodium chloride solution. Clean-up was performed using GC/PSA and C18 cartridges. In the case of livestock products and seafood, samples were extracted with a mixture of acetone and n-hexane, and the organic layer was collected. After acetonitrile-hexane partitioning, the extract was cleaned up using PAS and C18 cartridges. The gradient LC separation was performed on a C18 column with acetonitrile-water containing acetic acid as a mobile phase, and MS with positive ion electrospray ionization was used for detection. The average recoveries (n=5) of ipfencarbazone from 16 kinds of agricultural products, livestock products and seafood spiked at the MRLs or at the uniform limits (0.01 ppm) were 73-101%, and the relative standard deviations were 1.3-5.1%. The limit of quantitation of the developed method was 0.01 mg/kg for ipfencarbazone.
建立了一种采用液相色谱-串联质谱法测定农产品、畜产品和海产品中异戊乙净的方法。农产品用丙酮提取。取一份粗提取物用正己烷和饱和氯化钠溶液进行分配。使用石墨化碳黑/中性氧化铝和十八烷基硅烷键合硅胶柱进行净化。对于畜产品和海产品，样品用丙酮和正己烷的混合物提取，并收集有机层。经乙腈-正己烷分配后，提取物用primary-secondary amine（PAS）和十八烷基硅烷键合硅胶柱净化。在十八烷基硅烷键合硅胶柱上进行梯度液相色谱分离，以含乙酸的乙腈-水为流动相，采用正离子电喷雾电离质谱进行检测。在最大残留限量或统一限量（0.01 ppm）下加标的16种农产品、畜产品和海产品中，异戊乙净的平均回收率（n=5）为73%-101%，相对标准偏差为1.3%-5.1%。所建立方法对异戊乙净的定量限为0.01 mg/kg。
