酮洛芬注射液在乳牛体内的残留消除研究  

Determination of ketoprofen residual level in milk of lactating dairy cows using high performance liquid chromatography-tandem mass spectrometry

作　　者：王波[1] 曾艺元 邬嘉豪 沈祥广[1] 贺利民[1] 曾振灵[1] 曾东平[1] WANG Bo;ZENG Yi-yuan;WU Jia-hao;SHEN Xiang-guang;HE Li-min;ZENG Zhen-ling;ZENG Dong-ping(Guangdong Provincial Key Laboratory of Veterinary Pharmaceutics Development and Safety Evaluation/College of Veterinary Medicine.South China Agricultural University,Guangzhou 510642,China)

机构地区：[1]华南农业大学兽医学院广东省兽药研制与安全评价重点实验室

出　　处：《中国兽医科学》2020年第2期240-246,共7页Chinese Veterinary Science

基　　金：教育部创新团队发展计划资助项目（IRT13063)

摘　　要：为建立牛乳中酮洛芬的液相色谱-串联质谱(LC-MS/MS)检测方法,牛乳样品经甲醇提取,C18色谱柱分离,采用正离子模式,多反应监测,内标法定量。结果表明,牛乳中酮洛芬的检出限为1μg/kg,定量限为5μg/kg,在5~200μg/kg范围内线性关系良好,相关系数大于0.99。在25~100μg/kg添加水平的回收率为93.3%~107.5%,批内、批间相对标准偏差分别为1.72%~5.46%、1.13%~7.04%。该方法高效、灵敏、准确,可作为牛乳中酮洛芬的检测方法。选用20头健康的泌乳期荷斯坦乳牛,高产、低产各10头,以3 mg/kg剂量肌内注射给药,每天1次,连用3 d,分别于每次给药后第2、15小时采集乳样。每次给药后2 h牛乳中可检出酮洛芬,最高质量分数为(38.43±3.90)μg/kg,停药后15 h均未检出。所有时间点牛乳中酮洛芬质量分数的实测结果均低于加拿大规定的最高残留限量50μg/kg,建议弃乳期为0 d。To develop a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for the determination of ketoprofen in milk,milk samples were extracted with methanol,and separated on a C18 column.The analysis was performed under positive ionization and multiple reaction monitoring mode.The quantitation was performed by internal standard method.The results showed that the limits of detection was 1μg/kg and the limits of quantitation was 5μg/kg.Good linear-relationship existed between peak area and mass concentration of 5—200μg/kg with correlation coefficients higher than 0.99.The average recoveries at spiked concentration of 25—100μg/kg were in the range of 93.3%—107.5%.The relative standard deviations of intra-batch and inter-batch were in the range of 1.72%—5.46%,1.13%—7.04%,respectively.With the advantages of high efficiency,sensitivity,and accuracy,this method is suitable for the determination of ketoprofen in milk.Ketoprofen residue depletion was determined in milk from 20 healthy lactating dairy cows that intramuscularly administered 3 mg/kg three times at 24-h interval.The samples were collected during each milking(every 2 h and 15 h)for 3 consecutive days.The highest ketoprofen concentration in milk was observed 2 h after dosing(38.43μg/kg±3.90μg/kg).All observations were below the corresponding maximum residue limits(50μg/kg)in Canada.These results indicated that the withdrawal period in milk was 0 day.

关 键 词：酮洛芬 牛乳 残留 液相色谱-串联质谱 

分 类 号：S852.6[农业科学—基础兽医学]