作　　者： (梅英杰）; (史新宇）; (董瑾）; (朱西雷）; (张贞理）; (李德刚）;

机构地区： 山东理工大学化学工程学院,山东淄博255000 淄博市食品药品检验研究院,山东淄博255000

出　　处： 《食品与发酵工业》 2017年第8期240-245,共6页

摘　　要： 采用固相萃取法对鸡肉中氯霉素、四环素、金霉素和土霉素残留同时提取、净化、富集,并建立了用超高效液相色谱-串联质谱法对4种抗生素定性定量检测的分析方法。前处理部分采用含0.1%三氯乙酸的乙腈为提取溶剂,饱和了乙腈的正己烷溶液去除脂肪,超声波萃取2次;采用HLB固相萃取柱净化;色谱部分采用BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm),乙腈-0.2%甲酸水(含5 mmol/L乙酸铵)为流动相进行梯度洗脱。在最优条件下氯霉素、四环素、金霉素和土霉素在相应浓度范围内,线性良好,相关系数R2均大于0.999,其检出限分别为0.1、3.2、16.0、9.0μg/kg,日内、日间相对标准偏差(n=5)分别小于5.0%和10.0%,平均回收率为80.1%~92.5%。 A solid phase extraction column clean-up and ultra performance liquid chromatography - tandem mass spectrometry （UPLC-MS/MS） method was developed for simultaneous determination of chloramphenicol, tetracy-cline,chlortetracycline and oxytetracycline in chicken products. In the pre-treatment process,the sample was extracted with 0.1% trichloroaeetic acid-aeetonitrile and ultrasonic treatment twice, and fat was removed by aeetonitrile saturated n-hexane. HLB solid phase extraction column was used to purify. BEH Ct8 （2.1 mm × 50 mm, 1.7 μm） column was used and acetonitrile-0.2% formic acid （containing 5mmol/L ammonium acetate） was the gradient eluent. Under the above optimized conditions, chloramphenieol, tetracycline, chlortetracycline and oxytetracycline had a good linear correlation in the corresponding concentration ranges （R2 〉 0. 999）. The detection limits of four substances were 0.1, 3.2,16.0,9.0μg/kg,respectively. Intra-day and inter-day relative standard deviations （ n = 5 ） were less than 5.0% and 10.0% respectively. The average recoveries were between 80.1% and 92.5%.

关 键 词： 氯霉素 四环素 固相萃取 超高效液相色谱 串联质谱