摘要
针对鱼虾等水产品中的丙酸睾酮残留,以诺龙-D3为内标研究了气相色谱-质谱(GC/MS)检测技术。捣碎匀浆后的样品中加入内标诺龙-D3和饱和NaCl溶液混匀后,叔丁基甲醚超声提取,-80℃冷冻20min脱脂,SilicaSPE柱净化和柱前三甲基硅烷化后,进行GC/MS分析。选择离子监测(SIM)模式下,根据丙酸睾酮和诺龙-D3衍生物定量离子质量色谱图的峰面积比值,内标标准曲线法定量。实验结果表明,在0.025～1.0mg/L范围内,衍生物定量离子峰面积比值与丙酸睾酮浓度呈现良好线性关系,相关系数为0.9997;方法定量检出限为1.0μg/kg。当添加水平为1.0～10.0μg/kg时,回收率为74.1%～99.5%,相对标准偏差为3.0%～8.3%。通过对市场上8种鱼贝类的检测,进一步证明该法可实现对样品进行灵敏、准确的定性定量分析。
Using internal standard Nandrolone -D3, a gas chromatography-mass spectrometric method （GC-MS） was developed for the identification and quantitative determination of testosterone propionate residues in the muscle tissues of various fishery products. Homogenized tissue samples were added with Nandrolone-D3 and saturated sodium chloride solution were extracted by Tert-butyl ether under ultrasonication. Clean-up was carried out with freezing, followed by Silica solid phase extraction （SPE）. To enhance detection sensitivity, derivatization was achieved prior to GC-MS analysis with N-methyl-N-（ trimethylsilyl ）-trifluoroacetamide/iodotrimethylsilane/dithioeryth-ritol （ MSTFA-TM IS- DTE）. Quantitation using isotope-labeled internal standard was based on the ratio of peak area of testosterone propiohate derivative to peak area of internal standard Nandrolone-D3 derivative in the selected ion monitoring （SIM） mode with electron impact （El） source. The linearity ranged from 0.025 to 1.0 mg/L. The limit of quantitation （LOQ） was 1.0 μg/kg. At 1.0, 2.0, 10.0μg/kg spiked levels, the mean recoveries were 74.1% -99.5%, and the relative standard deviations were 3.0% - 8.3%. The application of this method was further demonstrated by analyzing various real samples from local markets.
出处
《中国渔业质量与标准》
2011年第3期55-61,共7页
Chinese Fishery Quality and Standards
基金
农业部行业标准项目(农财发2008[74]号)
现代农业产业技术体系专项资金资助(CARS-50-G09)
关键词
丙酸睾酮
水产品
气相色谱-质谱
testosterone propionate
fishery products
gas chromatography-mass spectrometry
