摘要
建立牛奶中四环素族抗生素残留的高效液相色谱法。方法:样品5g经20ml EDTA-Mcllvain缓冲液提取,离心后取5ml上清液于预平衡的Sep-Pak WatersTM Sep-Pak? C18 固相萃取柱净化,用10mmol/L的草酸甲醇溶液洗脱,并于40℃用N2浓缩仪吹干,流动相0.5ml溶解残渣进行HPLC分析。结果:标准校准曲线在0.05～1.0mg/L的范围内,相关系数r>0.99。牛奶中土霉素、四环素一金霉素和强力霉素的定量检测限(LOQ)依次是0.025、0.025、0.05、和0.05mg/L;添加水平分别为0.1、0.1、0.2和0.2mg/L时,样品加标回收率为84%～110%,RSD<10%。结论:方法简便可行、净化效果好、检测灵敏度、准确度及精密度均满足检测要求。
Objective: To establish a SPE-HPLC method for the simultaneous determination of multi-tetracyclines(TCs) residues in milk. Method: The TCs in 5g milk sample was extracted with 20ml EDTA-Mcllvain buffer, then after centrifugation, the 5ml supernatant liquid was loaded on an preconditioned SPE Sep-Pak? C18 cartridge. The TCs was eluted with 3ml 10mmol/L oxalic acid methanol following the rinse clean-up. Then eluant was evaporated with N2 to dryness at 40℃, and the residues was redissolved with 0.5ml HPLC flow phase and detected with HPLC method. Results: The calibration curve was linear in the range 0.05-1.0mg/ L and r>0.99. The limit of quantification (LOQ) was 0.025, 0.025, 0.05 and 0.05mg/L respectively for oxytetracyline, tetracycline, chlortetracycline and doxytetracyline residues in milk, and at the corresponding spike level 0.1, 0.1, 0.2 and 0.2mg/L respectively. The recovery rates were 84%￣110% and RSD<10%. Conclusion:The method was applicable for the detection of TCs residues in milk. The clean-up effect, sensitivity, accuracy and prevision have all met the analysis requirement.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2005年第3期202-204,共3页
Food Science
