同位素稀释高压液相色谱-串联质谱法测定 鱼虾中丙酸睾酮残留量

Determination of testosterone propionate residues in fish and shrimp by high pressure liquid chromatography-tandem mass spectrometry with isotope dilution

中文关键词:  丙酸睾酮  鱼虾  低温冷冻  高速离心  高压液相色谱-串联质谱

英文关键词:Qingdao  trimethylamine N-oxide (TMAO)  aquatic products  ion chromatography

中文摘要:

      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0.5 μg/kg。当添加水平为0.5~10.0 μg/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。

英文摘要:

      Objective A rapid, specific and highly sensitive method for the determination of testosterone propionateresidue in fish and shrimp was developed using high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Homogenized tissue samples which were added with nandrolone-D3 were extracted by tert-butyl ether under ultrasonication and cleaned up with freezing and high-speed centrifugation. The target compounds were separated on Eclipse Plus C18 (100 mm×2.1 mm, 3 μm) using acetonitrile-0.1% formic acid as mobile phase at a flow rate of 0.3 mL/min, and detected qualitatively and quantitatively in selected reaction monitoring(SRM) under positive mode. Results The linearity ranged from 0.5 to 100 ng/mL and correlation coefficient was 0.9989. The limit of quantitation (LOQ) was 0.5 μg/kg. At the spiked levels of 0.5, 1.0, 2.0 μg/kg and 10.0 μg/kg, the average recoveries ranged from 71.2% to 104.5%. The relative standard deviations were between 2.26% and 5.65%. Conclusion The method is simple, sensitive and accurate for detecting the testosterone propionate in aquatic products.