摘要
建立了分散液液微萃取(DLLME)技术进行样品前处理,高效液相色谱(HPLC)法测定猪肾脏中土霉素(OTC)、四环素(TC)、金霉素(CTC)3种四环素类抗生素(TCs)残留量的方法。考察了分散剂种类、离子液体用量、分散剂用量、样品溶液p H值、萃取时间、盐效应等因素对萃取效率的影响。优化后的实验条件为:以丙酮为分散剂,离子液体([BMIM]PF6)用量为50μL,分散剂用量为140μL,样品溶液p H值为3.0,萃取时间为15 min,不添加盐。该方法在0.1~10.0 mg/L范围内线性关系良好(r2≥0.999 5),土霉素、四环素和金霉素的相对标准偏差(RSD)为2.2%~3.1%,检出限(LOD)为54~93μg/L,富集倍数为7.0~27.8,且样品的加标回收率达99.5%~101.1%。该法准确度和精密度均满足分析方法的要求,实现了对猪肾脏中土霉素、四环素、金霉素3种四环素类抗生素残留量的快速、绿色、灵敏和准确检测。
A method was established for the determination of three tetracycline antibiotics（TCs） residues such as oxytetracycline,tetracycline and chlortetracycline in pig kidney by high performance liquid chromatography（HPLC） coupled with dispersive liquid-liquid microextraction（DLLME）.The influences of dispersant type,amount of ionic liquid,amount of dispersant,pH of sample solution,extraction time and effect of salts on extraction efficiency were investigated.The optimum experimental conditions were as follows：using acetone as the dispersant,a 50 μL ionic liquid（［BMIM］ PF6）,a 140 μL dispersant,a pH 3.0 sample solution,a 15 min of extraction time and no salt.The results showed that this method provided a wide linearity in the range of 0.1-10.0 mg/L with correlation coefficients no less than 0.999 5.The relative standard deviations（RSDs） were 2.2%-3.1%for oxytetracycline,tetracycline and chlortetracycline.The detection limits（LOD） were in the range of 54-93 μg/L with the enrichment folds of 7.0-27.8,and the recoveries were 99.5%-101.1%.It was found that the accuracy and precision could meet the requirements for the rapid,green,sensitive and accurate detection of oxytetracycline,tetracycline and chlortetracycline residues in pig kidney.
出处
《分析测试学报》
CAS
CSCD
北大核心
2017年第11期1352-1356,共5页
Journal of Instrumental Analysis
基金
国家自然科学基金(21265002)
江西省科级支撑计划项目(20151BBG70048)
关键词
离子液体
分散液液微萃取
高效液相色谱
四环素类抗生素
猪肾脏
ionic liquid（IL）
dispersive liquid-liquid microextraction（DLLME）
high performance liquid chromatography（HPLC）
tetracycline antibiotics（TCs）
pig kidney
