养殖三疣梭子蟹中甲基法尼酯的GC／MS分析

建立了人工养殖三疣梭子蟹（Portunus trituberculatus）淋巴和肌肉中甲基法尼酯的毛细管气相色谱．质谱联用检测法。向淋巴或冷冻干燥后的肌肉样品中加入十九烷酸甲酯作为定量内标物，淋巴中加入0．9％NaCl和乙腈后用正己烷提取；肌肉冷冻干燥后用正己烷提取，浓缩定容后用EI源在SIM检测模式下进行检测．结果表明：甲基法尼酯与内标物十九烷酸甲酯在SPB—1柱上得到良好的分离，方法在5．00～200．00ng·mL^-1。浓度范围内线性关系良好，相关系数为0．99995，方法的最低检测限3．27pg．淋巴和肌肉中甲基法尼酯平均回收率分别达到95．32％和88．37％，标准相对偏差分别为5．71％和7．94％．对采自浙江宁波象山港养殖三疣梭子蟹进行分析测定，甲基法尼酯在血清中含量在15．11～145．23ng·mL^-1。范围内，而肌肉中则在3．23～10．32ng·g^-1范围内．

Determination of Methyl Farnesoate in Cultured Portunus Trituberculatus by GC/MS

An analytical method on sensitivity of methyl farnesoate in lymph and muscle of cultured Portunus trituberculatus is introduced using capillary gas chromatography-mass spectrometry. After nonadeeanoic acid methylester is added to lymph and frozen drying muscle as inner standard, and 0.9% NaCl and acetonitrile are added to lymph, methyl farnesoate can be extracted with n-hexane effectively, and determined using EI-SIM-MS after concentration. The results indicate that methyl farnesoate and the inner standard can be separated from each other on SBP-1 column with sharp peak. The linearity is agreeable from 5.00 to 200.00ng.mL^-1 and relative coefficient is found to be 0.999 95, with low detection limit of 3.27 pg. The average recovery rate in lymph and muscle is 95.32% and 88.37%, respectively, and the standard deviation reads 5.71% and 7.94%, respectively. This method is applied to determine the methyl farnesoate at different stages of P trituberculatus, coming up with the results of 15.11-145.23 ng.mL^-1 in lymph and 3.23-10.32 ng.g^-1 in muscle.