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大甲基法尼酯是甲壳类动物体内的一种激素,在早期发育阶段具有改变形态的生物活性,并对繁殖起调控作用.本论文发展了一种基于正相高效液相色谱法纯化、气相色谱-质谱联用仪分析的综合分析方法.以非生物活性异构体反式-顺式-大甲基法尼酯(C-T-MF)作为内标物并用无分流注射法进样,采用电子撞击电离源电离后检测.利用无分流注射模式检测时,气相色谱-质谱联用仪的T-T-MF检出下限为100 pg/(次.柱).若取血淋巴样品4 mL,从最终25μL提取物中注入2μL,此方法的检出下限为0.3 ng/mL.在样品制备第一步(包括溶剂萃取、高效液相色谱纯化、气相色谱-质谱联用仪分析)就加入25 ng T-T-MF的条件下,总回收率为79%(RSD=5%,n=5).这种综合分析方法已被成功地应用于测定甲壳类动物血淋巴中T-T-MF的含量,如龙虾(Homarus americanus)、墨吉尔虾(Fennero peneaus merg-uiensis)、小龙虾(Procambarus clarkii).
Methyl farnese, a hormone in crustacean, has the biological activity of morphological changes in the early developmental stages and plays a regulatory role in reproduction.In this paper, a new method based on normal phase high performance liquid chromatography (HPLC) Gas chromatography-mass spectrometry (GC-MS / MS) analysis was performed using non-bioactive isomer trans-cis-megamethyl farnesyl ester (CT-MF) Electron impact ionization ionization was detected after ionization.The detection limit of TT-MF in gas chromatography-mass spectrometry was 100 pg / (times.column) when using splitless injection mode.If 4 mL hemolymph samples were taken, 25 μL of extract was injected with 2 μL and the limit of detection for this method was 0.3 ng / mL For the first step of the sample preparation (including solvent extraction, HPLC, gas chromatography-mass spectrometry analysis), 25 ng TT -MF, the overall recovery was 79% (RSD = 5%, n = 5) .This comprehensive analysis has been successfully applied to the determination of TT-MF in the hemolymph of crustaceans such as lobster ( Homarus americanus, Fennero peneaus merg-uiensis, Procambarus clarki i).