Development of a Candidate Reference Method for the Simultaneous Quantitation of the Boar Taint Compounds Androstenone, 3伪-Androstenol, 3尾-Androstenol, Skatole, and Indole in Pig Fat by Means of Stabl

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• 作者：Jochen Fischer ; Paul W. Elsinghorst ; Mark Bu虉cking ; Ernst Tholen ; Brigitte Petersen ; Matthias Wu虉st
• 刊名：Analytical Chemistry
• 出版年：2011
• 出版时间：September 1, 2011
• 年：2011
• 卷：83
• 期：17
• 页码：6785-6791
• 全文大小：781K
• 年卷期：v.83,no.17(September 1, 2011)
• ISSN：1520-6882

文摘

The steroidal pig pheromones androstenone (5伪-androst-16-en-3-one), 3伪-androstenol (5伪-androst-16-en-3伪-ol), and 3尾-androstenol (5伪-androst-16-en-3尾-ol) as well as the heterocyclic aromatic amines skatole and indole, originating from microbial degradation of tryptophan in the intestine of pigs, are frequently recognized as the major compounds responsible for boar taint. A new procedure, applying stable isotope dilution analysis (SIDA) and headspace solid-phase microextraction鈥揼as chromatography/mass spectrometry (HS-SPME鈥揋C/MS) for the simultaneous quantitation of these boar taint compounds in pig fat was developed and validated. The deuterated compounds androstenone-d₃, 3尾-androstenol-d₃, skatole-d₃, and indole-d₆ were synthesized and successfully employed as internal standards for SIDA. The new procedure is characterized by a fast, simple, and economic sample preparation: methanolic extraction of the melted fat followed by a freezing and an evaporation step allows for extraction and enrichment of all five analytes. Additional time-consuming cleanup steps were not necessary, as HS-SPME sampling overcomes fat-associated injector and column contamination. The method has been validated by determining intra- and interday precision and accuracy as well as the limit of detection (LOD) and limit of quantitation (LOQ). Additionally, a cross-validation for androstenone, skatole, and indole was carried out comparing the results of 25 back fat samples obtained simultaneously by the new SIDA鈥揌S-SPME鈥揋C/MS procedure with those obtained in separate GC/MS and high-performance liquid chromatography fluorescence detection (HPLC-FD) measurements. The cross-validation revealed comparable results and confirms the feasibility of the new SIDA鈥揌S-SPME鈥揋C/MS procedure.