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采用超高效液相色谱-串联质谱法测定头孢氨苄残留量:猪体内残留消除研究。

Determination of cephalexin residual level using ultra-high-performance liquid chromatography-tandem mass spectrometry: Residue depletion study in swine.

机构信息

Beijing Advanced Innovation Center for Food Nutrition and Human Health, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.

Shenzhen Center for Disease Control and Prevention, Shenzhen 518020, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Aug 15;1124:233-238. doi: 10.1016/j.jchromb.2019.06.003. Epub 2019 Jun 5.

Abstract

An ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed to analyze cephalexin in swine tissues, urine, and feces. Samples were extracted with 1% sulfuric acid, followed by purification using MCX cartridges. Mean recoveries were 95.4%-100.7% with inter-day relative standard deviations of <8.6%. The quantitation limit was 5 μg/kg for fat and urine, and 10 μg/kg for muscle, liver, kidney, and feces. Cephalexin residue depletion was determined using 32 healthy pigs, randomly divided into eight (seven treated and one control) groups. Treated groups were intramuscularly administered 10 mg/kg b.w. five times at 24-h intervals and euthanized 6 h and 1, 2, 3, 5, 7, and 10 days after the last injection. Cephalexin was eliminated rapidly in swine muscle, liver, fat, and feces. The highest concentrations among edible organs were detected in the kidney. Moreover, the longest elimination period of cephalexin in swine was determined in urine. These results indicated that kidney and urine were likely target matrices for cephalexin residue detection in swine.

摘要

建立了一种超高效液相色谱-串联质谱法,用于分析猪组织、尿液和粪便中的头孢氨苄。样品用 1%硫酸提取,然后用 MCX 小柱净化。日内相对标准偏差<8.6%,平均回收率为 95.4%-100.7%。脂肪和尿液的定量限为 5μg/kg,肌肉、肝脏、肾脏和粪便的定量限为 10μg/kg。采用 32 头健康猪进行头孢氨苄残留消除试验,随机分为 8 组(7 个处理组和 1 个对照组)。处理组肌肉注射 10mg/kg b.w.,每 24 小时一次,共 5 次,最后一次注射后 6 小时和 1、2、3、5、7 和 10 天安乐死。头孢氨苄在猪肌肉、肝脏、脂肪和粪便中迅速消除。在可食用器官中,肾脏中检测到的头孢氨苄浓度最高。此外,尿液中头孢氨苄的消除半衰期最长。这些结果表明,肾脏和尿液可能是猪中头孢氨苄残留检测的靶基质。

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