METHOD FOR QUANTITATIVE-DETERMINATION OF THE 4 KNOWN JUVENILE HORMONES IN INSECT TISSUE USING GAS CHROMATOGRAPHY-MASS SPECTROSCOPY
METHOD FOR QUANTITATIVE-DETERMINATION OF THE 4 KNOWN JUVENILE HORMONES IN INSECT TISSUE USING GAS CHROMATOGRAPHY-MASS SPECTROSCOPY
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DOI：
10.1016/s0021-9673(00)81664-7
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发表时间：
1981-01-01
期刊：
影响因子：
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通讯作者：
SCHOOLEY, DA
中科院分区：
文献类型：
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作者：
BERGOT, BJ;RATCLIFF, M;SCHOOLEY, DA
描述了一种快速、特异性和灵敏的方法，用于提取、纯化和定量测定昆虫组织中三种已知的保幼激素，该方法使用电子轰击模式下的组合气相色谱-质谱法 (GC-MS) 和选择离子监测 (SIM) 进行检测。第四种新的、天然存在的保幼激素以这种方式被检测到（并随后通过其他方法鉴定）。生物材料初步提取后，利用非水反相和氧化铝微型柱色谱的快速高效纯化序列可快速实现 103-104 的纯化因子。通过 10,11-环氧化物部分的酸催化甲烷-d3-水解进行衍生化分析，然后对所得 11-甲氧基-d3-10-羟基（甲氧基醇）衍生物进行液相色谱分离，完成样品后处理。然后通过 GC-MS (SIM) 直接分析甲氧基醇。在提取过程中添加氚标记的类似物作为内标，这样可以确定每个样品的回收率，同时确保定量准确性。回收率为 75-80%，通常可实现每克组织 10-40 pg 的检测限。
A rapid, specific, and sensitive method is described for the extraction, purification, and quantitative determination of the three known juvenile hormones in insect tissue, using combined gas chromatography—mass spectroscopy (GC—MS) in the electron impact mode with selected ion-monitoring (SIM) for detection. A fourth, new, naturally occuring juvenile hormone was detected (and subsequently identified by other means) in this way. After initial extraction of biological material, a fast and efficient purification sequence utilizing non-aqueous reversed-phase and alumina mini-column chromatography achieves quickly a 103–104purification factor. Derivatization for analysis by acid-catalyzed methan-d3-olysis of the 10,11-epoxide moiety, followed by liquid chromatography separation of the resultant 11-methoxy-d3-10-hydroxy (methoxyhydrin) derivatives, completes the sample work-up. The methoxyhydrins are then directly analyzed by GC—MS (SIM). A tritium-labeled analogue is added during the extraction as an internal standard, which allows determination of recovery for each sample and simultaneously assures quantitative accuracy. Recoveries are 75–80%, and detection limits of 10–40 pg per gram of tissue are normally achievable.