摘要
为了评估磺胺类药物在水产品基质中的稳定性以及检测结果的影响因素,开展了磺胺类药物检测质量控制技术研究。本研究模拟从样品制备到检测全过程中的环境条件,采用对虾基质加标方法,分析了3种加标浓度(40、50、70μg/kg)的磺胺类药物残留在4种储藏条件下(对样品进行反复冻融和低温保藏等处理)的稳定性;同时,比较了水产品中磺胺类药物残留常用的2种检测方法:农业部958号公告-12-2007(液相色谱法)和农业部1077号公告-1-2008(液相色谱串联质谱法)对检测结果的影响。结果表明:磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺邻二甲氧嘧啶不同浓度的加标回收率为71.2%~98.9%,各试验组别之间不存在显著性差异,水产品中磺胺药物的残留稳定性较强。2种检测方法均能满足检测要求,样品检测前需要遵循样品的实际情况及方法的适用范围合理选择检测方法,确保检测结果准确可靠。
In order to assess the stability of sulfa drug in aquatic organization and factors that affect the test results, quality control testing technology research had been carried out. The environmental conditions from sampling to test process had been simulated. Shrimp spiked samples in 3 concentrations (40, 50, 70 μg/kg) under 4 different storage conditions (treated under repeated freezing, thawing and cryopreservation processing) were tested. At the same time, inter-laboratory comparison of 2 designated detection methods had been carried out: the Ministry of Agriculture Bulletin No.958-12-2007 (reverse phase high-performance liquid chromatography) and the Ministry of Agriculture Bulletin No.1077-1-2008 (liquid chromatography tandem mass spectrometry). The results showed that, there was no significant difference between the experimental groups, the recoveries of sulfadiazine, sulfa-merazine, sulfa-methazine, sulfadimoxine in different concentrations was between 71.2%-98.9%, the stability of 4 sulfa drugs in aquatic organizations were strong. 2 detection methods could meet the test requirements, reasonable choice of detection method before inspectionshould follow the actual needs of samples and methods applicable range, to ensure accurate and reliable detection results.
出处
《中国农学通报》
CSCD
2014年第5期53-60,共8页
Chinese Agricultural Science Bulletin
基金
国家自然科学基金项目"鱼类谷胱甘肽对麻痹性贝毒氧化胁迫的响应机制"(41106109)
中央级基本科研业务费项目"虾夷扇贝质量安全形成过程"(20603022012019
20603022011004)
关键词
磺胺
检测方法
样品稳定性
sulfonamides
detection methods
samples stability