摘要
建立了鱼粉中氯霉素和β-受体激动剂(克仑特罗、沙丁胺醇)兽药残留标准物质的研制与定值方法。通过对药物在河鲫鱼(Carassius auratus)体内的代谢研究,对含有药物残留的肌肉组织进行匀浆、冷冻干燥和均匀化后加工处理,按照最小取样量进行真空包装后共得400袋。随机取其中100袋分为10组,每组随机取1袋做组间均匀性检验,随机取1组做组内均匀性检验。分析测试结果经过F检验和t检验,在95%置信区间内。经过1年时间,在-18、4和25℃3种保存条件下稳定性检验,测试结果表明标准物质特征值变化在不确定度范围内。制备的鱼粉标准物质采用同位素稀释液相色谱-串联质谱法,与国内8个具有一定分析资质的实验室进行协同定值。定值后的样品中氯霉素、克伦特罗和沙丁胺醇浓度的特征值分别为11.8、9.9和12.8μg/kg,相对不确定度分别为26.3%、9.1%和18.0%。本研究对进一步完善药物残留标准物质的制备具有参考价值。
A methodology regarding preparation and certification of reference material for chloramphenicol and β-agonists（clenbuterol and salbutamol）in fish powder was presented. The reference materials were based on breeding and metabolic research on river crucian Carassius auratus in Shanghai with respect to the related veterinary drugs. About 400 bags of samples were obtained from the fortified muscles of river crucian according to the minimum weight for analysis by the procedure of homogenation and cryodesiccation. The residual concentration of fish powder was determined by isotope dilution liquid chromatography coupled to tandem mass spectrometry. A cooperative certification was conducted with 8 qualified laboratories to provide reference materials in fish powder with fortified level of 11. 8 μg/kg （ chloramphenico ）, 9.9 μg/kg （ clenbuterol ） and 12.8 μg/kg（salbutamol） respectively, as well as a relative uncertainty of 26.3% for chloramphenicol, 9.1% for clenbuterol and 18.0% for salbutamol respectively. The materials were intended for use in the method vali- dation and quality control regarding chloramphenicol and β-agonist analysis within laboratory of veterinary drug inspection.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2008年第9期1221-1227,共7页
Chinese Journal of Analytical Chemistry
基金
质检总局重点攻关项目(No.2003IK041)
上海市应对技术性贸易壁垒项目(No.05TBT008)资助
关键词
食品安全
标准物质
氯霉素
β-受体激动剂
鱼粉
Food safety, reference material, chloramphenicol,β-agonist, fish powder
