Saito Shizuka, Sakai Takatoshi, Nemoto Satoru, Matsuda Rieko
National Institute of Health Sciences, Tokyo, Japan.
Shokuhin Eiseigaku Zasshi. 2011;52(5):294-8. doi: 10.3358/shokueishi.52.294.
A sensitive and selective analytical method for the determination of the rodenticide pindone in animal products, fishery products, and honey by LC-MS/MS was developed. Pindone was extracted with acidified acetone, and the crude extract was purified by liquid-liquid partitioning, followed by silica gel and ODS column chromatography. LC separation was performed on an ODS column with methanol/water containing ammonium acetate as the mobile phase, and detection was carried out using tandem mass spectrometry (MS/MS) with electrospray ionization (ESI) in the negative mode. The average recoveries from fortified bovine muscle, bovine liver, bovine fat, chicken muscle, salmon, eel, freshwater clam, egg, milk, and honey spiked at 0.001 mg/kg were in the range of 76-92%, and the relative standard deviations were 4-8%. The limit of quantitation (S/N≥10) of the developed method was 0.001 mg/kg for all the tested foods.
建立了一种灵敏且选择性好的液相色谱-串联质谱法（LC-MS/MS），用于测定动物产品、水产品及蜂蜜中的杀鼠剂茚满二酮。茚满二酮用酸化丙酮提取，粗提物经液-液分配净化，再经硅胶柱和十八烷基硅烷键合硅胶柱（ODS柱）色谱法净化。液相色谱分离在ODS柱上进行，以含醋酸铵的甲醇/水为流动相，采用串联质谱（MS/MS）、电喷雾电离（ESI）负离子模式进行检测。在0.001 mg/kg加标水平下，该方法在牛肌肉、牛肝、牛脂肪、鸡肌肉、三文鱼、鳗鱼、淡水蛤、鸡蛋、牛奶及蜂蜜中的平均回收率为76%92%，相对标准偏差为4%8%。该方法对所有被测食品的定量限（S/N≥10）均为0.001 mg/kg。
