鲫组织中伊维菌素含量的检测方法
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上海市教委理科重点项目(07ZZ132);上海市教委重点学科建设项目(J50701);上海海洋大学博士启动基金项目(B8201060312)


Research on the method for ivermectin determination in different crucian tissues
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    摘要:

    采用反相高效液相色谱分离、紫外检测器检测,建立了鲫血液、肌肉、肝胰脏、肾脏及性腺组织中伊维菌素(IVM)残留的检测方法。将匀浆后的鲫组织用乙酸乙酯提取,离心后取上清液于45 ℃下氮气吹干,用甲醇-水(4∶1,V/V)混合液溶解残渣,加正己烷,漩涡振荡后离心,取下清液经0.22 μm的滤膜过滤后,进样20 μL进行分析,检测波长为245 nm,外标法定量。结果表明:伊维菌素在血浆和肌肉中的检出限分别为7.5 μg/L和7.0 μg/kg;肌肉、肝胰脏、肾脏及性腺中IVM为0.025~1.00 mg/kg,血液中为0.025~1.00 mg/L时,色谱峰峰高与浓度呈良好的线性相关。各组织中IVM的平均回收率为(90.09±6.54)%~(97.77±5.91)%,平均批内RSD为(2.55±1.78)%~(3.99±1.55)%,平均批间RSD为(4.18±3.97)%~(6.01±2.54)%。对鲫以0.4 mg/kg(药量/体重)剂量单次口灌给药后,用该方法进行残留检测,结果发现:25 ℃水温条件下,鲫肌肉中伊维菌素的休药期不得少于15 d。

    Abstract:

    A method using reversed phase high performance liquid chromatography with UV detection has been developed for the determination of ivermectin residues in crucian blood,muscle,hepatopancreas,kidney and gonad tissues.Homogenized crucian tissues were extracted with ethylacetate prior to centrifugation.The supernatants were evaporated to dryness at 45 ℃ with nitrogen.The residues were dissolved with the mixture of methanolwater(4∶1,V/V)and defatted with hexane.After centrifugation,the underlayers were filtrated with 0.22 μm filter and then 20 μL filtrates were detected by reverse phase high performance liquid chromatography with 245 nm detection wavelength.Its method detection limit was 7.5 μg/L and 7.0 μg/kg in plasma and muscle respectively.The good linear range was 0.025-1.00 mg/kg in crucian muscle,hepatopancreas,kidney,gonad tissues and 0.025-1.00 mg/L in plasma.In different tissues,the average withinbatch and the betweenbatch standard deviations of this method are(2.55±1.78)%-(3.99±1.55)% and(4.18±3.97)%-(6.01±2.54)% respectively,with an average recovery of(90.09±6.54)%-(97.77±5.91)%.After a single oral administration of 0.4 mg/kg body weight,we detected ivermectin residues in crucian muscle tissues with this method.When the water temperature is 25 ℃,we found that the freedrug period of crucian muscle tissues should not be less than 15 days.

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彭章晓,何琳,江敏,吴昊,杨李.鲫组织中伊维菌素含量的检测方法[J].水产学报,2010,34(6):784~791

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  • 收稿日期:2010-01-22
  • 最后修改日期:2010-04-09
  • 录用日期:2010-04-12
  • 在线发布日期: 2010-06-10
  • 出版日期: 2010-06-15