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目的采用高压液相色谱-串联质谱(high pressure liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)快速检测鱼虾等水产品中丙酸睾酮残留。方法向捣碎匀浆后的样品中加入内标诺龙-D3混匀后,叔丁基甲醚超声提取,-80℃冷冻30 min后12000 r/min离心净化。以Eclipse Plus C18为色谱分离柱,以乙腈-0.1%甲酸水溶液为流动相,流速为0.3 mL/min,采用三重四极杆质谱在正离子模式下进行选择反应离子监测。结果丙酸睾酮在0.5~100 ng/mL范围内呈线性关系,相关系数为0.9989;方法定量限为0.5μg/kg。当添加水平为0.5~10.0μg/kg时,平均回收率为71.2%~104.5%,相对标准偏差为2.26%~5.65%。结论该方法操作简单、快速、灵敏度高,适用于快速检测水产品中丙酸睾酮的残留量。
OBJECTIVE To rapidly detect testosterone propionate residues in fish and fishery products by high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). Methods After the homogenized sample was added with the internal standard nandrolone-D3, the mixture was triturated with tert-butyl methyl ether and then centrifuged at 12000 r / min for 30 min at -80 ℃. Eclipse Plus C18 was used as the chromatographic column. The mobile phase was acetonitrile-0.1% formic acid aqueous solution and the flow rate was 0.3 mL / min. Triple ion quadrupole mass spectrometry was used to monitor selective ionization in positive ion mode. Results Testosterone propionate showed a linear relationship in the range of 0.5-100 ng / mL with a correlation coefficient of 0.9989. The limit of quantification was 0.5 μg / kg. The average recoveries ranged from 71.2% to 104.5% and the relative standard deviations (RSDs) ranged from 2.26% to 5.65% at 0.5-10.0 μg / kg. Conclusion The method is simple, rapid, sensitive and suitable for rapid detection of testosterone propionate residues in aquatic products.