摘要
本研究旨在建立一种同时准确测定饲料中4种林可胺类药物(林可霉素、克林霉素、克林霉素磷酸酯和吡利霉素)的方法。饲料中林可胺类药物用甲醇-0.1 mol/L磷酸氢二钾(8∶2,体积比)缓冲溶液提取,提取液经混合型强阳离子交换固相萃取小柱净化,采用C18色谱柱分离,流动相为0.1%甲酸溶液和乙腈,梯度洗脱,以电喷雾离子源(ESI)正离子扫描方式,在多反应监测(MRM)模式下进行测定,外标法定量。结果表明:本研究建立的固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)法对饲料中林可胺类药物检出限为10μg/kg,定量限为40μg/kg;4种林可胺类药物在1~200μg/L浓度范围内,线性关系良好,相关系数(R2)均大于0.99;在4个浓度水平(40μg/kg、400μg/kg、4 mg/kg和100 mg/kg)下进行添加试验,林可胺类药物的回收率为81.5%~107.6%,相对标准偏差(RSD)为1.4%~9.8%。由此可见,本研究建立的SPE-UPLC-MS/MS法灵敏、可靠,可应用于饲料中4种林可胺类药物的准确测定。
The aim of this study was to establish a simultaneous and accurate method for the determination of 4 lincosamides(lincomycin,clindamycin,clindamycin phosphateand and pirlimycin)in feed.Lincosamides were extracted from feed by methanol⁃0.1 mol/L dipotassium hydrogen phosphate(8∶2,volume ratio)buffer solution,and the extracted solution was purified by mixed strong cation exchange solid phase extraction car⁃tridge.Then the lincosamides were separated by a C18 column with gradient elution using 0.1%formic acid so⁃lution and acetonitrile as mobile phase and finally confirmed and quantified by external standard method in mul⁃tiple reaction monitoring(MRM)mode with electrospray ion source(ESI)positive ion scanning mode.The results showed that the limits of detection and quantitation of lincosamides in feed were 10 and 40μg/kg re⁃spectively by solid phase extraction⁃ultra⁃high performance liquid chromatography⁃tandem mass spectrometry(SPE⁃UPLC⁃MS/MS)method built in this study;the linear relationship was good in the concentration range of 1 to 200μg/L,and the correlation coefficient(R2)was greater than 0.99;at the four spiked levels(40μg/kg,400μg/kg,4 mg/kg and 100 mg/kg),the recovery rate of lincosamides was 81.5%to 107.6%,and the relative standard deviation(RSD)was 1.4%to 9.8%.As a result,the SPE⁃UPLC⁃MS/MS method built in this study was sensitive and reliable for the accurate determination of 4 lincosamides in feed.
作者
王凤芹
开丽霞
程远之
汪以真
WANG Fengqin;KAI Lixia;CHENG Yuanzhi;WANG Yizhen(Key Laboratory of Animal Nutrition and Feed Science of Zhejiang Province,Key Laboratory of Animal Nutrition and Feed Science in Eastern China,Ministry of Agriculture and Rural Affairs,Key Laboratory of Molecular Animal Nutrition,Ministry of Education,College of Animal Sciences,Zhejiang University,Hangzhou 310058,China)
出处
《动物营养学报》
CAS
CSCD
北大核心
2023年第6期3978-3990,共13页
CHINESE JOURNAL OF ANIMAL NUTRITION
基金
现代农业生猪产业体系(CARS⁃36)。
关键词
固相萃取
超高效液相色谱-串联质谱法
饲料
林可胺类药物
solid phase extraction
ultra⁃high performance liquid chromatography⁃tandem mass spectrometry
feed
lincosamides
