Takahashi Kunihiko, Matsumoto Ryuji, Nemoto Satoru, Matsuda Rieko
Saitama Institute of Public Health, Sakura-ku, Saitama-shi, Saitama, Japan.
Shokuhin Eiseigaku Zasshi. 2011;52(1):47-50. doi: 10.3358/shokueishi.52.47.
A simple determination method of hydramethylnon in agricultural products by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. The sample was homogenized with phosphoric acid and extracted with acetone. An aliquot of crude extract was re-extracted with hexane and sat. NaCl solution. In the case of tea leaf, solidification processing using ammonium chloride and phosphoric acid was performed before re-extraction with hexane. Clean-up was performed using a silica-gel mini column (500 mg). The LC separation was performed on a C18 column using methanol-water (8 : 2) containing 10 mM ammonium acetate as the mobile phase and MS detection with positive ion electrospray ionization. The calibration curve was linear between 0.002-0.2 µg/mL of hydramethylnon. Recoveries (n=5) of hydromethylnon from 10 kinds of agricultural products fortified at 0.01 µg/g (0.05 µg/g for pineapple) were 82-110%, and their relative standard deviations were 2-12%.
建立了一种用液相色谱-串联质谱法（LC-MS/MS）测定农产品中氟蚁腙的简单方法。样品用磷酸匀浆，并用丙酮萃取。取一份粗提物用己烷和饱和氯化钠溶液再萃取。对于茶叶，在用己烷再萃取之前，先用氯化铵和磷酸进行固化处理。使用硅胶微型柱（500 mg）进行净化。在C18柱上进行LC分离，以含10 mM乙酸铵的甲醇-水（8:2）为流动相，并采用正离子电喷雾电离进行MS检测。氟蚁腙的校准曲线在0.002-0.2 µg/mL之间呈线性。在10种添加了0.01 µg/g（菠萝为0.05 µg/g）氟蚁腙的农产品中，氟蚁腙的回收率（n=5）为82-110%，其相对标准偏差为2-12%。
