超高效液相色谱法检测猪肉中麻保沙星残留  

Detection of marbofloxacin residues in pork using ultra performance liquid chromatography

作　　者：赵莉[1] 韩合敬 郝智慧[1] 王仕文[1] 杨芬芳[1] 黄亭亭[1] 

机构地区：[1]青岛农业大学化学与药学学院,山东青岛266109

出　　处：《黑龙江畜牧兽医》2016年第12期267-270,共4页Heilongjiang Animal Science And veterinary Medicine

基　　金：国家自然科学基金项目(31402256);农业部公益性行业专项项目(201303038-8);山东省高等学校科技计划项目(J13LM09)

摘　　要：为了检测猪肉中麻保沙星残留，试验采用一种快速、高效的超高效液相色谱（UPLC）法，以氧氟沙星为内标，样品经三氯甲烷提取，50℃吹干，流动相溶解，正己烷除脂，紫外检测器检测，色谱柱为Waters ACQUITY BEH RP18柱（2．1mm×50mm，1．7μm），流动相为0．2％三氟乙酸（A）：乙腈（B）=82：18。结果表明：线性范围为10—1000μg/kg（r=0．9994），检出限为5μg／kg，定量限为10μg/kg，在50，150，300μg／kg3个浓度水平进行添加试验，平均回收率为85．80％～103．20％，批内相对标准偏差为2．1％-3．8％，批间相对标准偏差为2．9％-4．7％。此方法操作简单、灵敏度高，可用于相关药物的残留检测。To detect marbofloxacin residues in pork, a fast and efficient ultra performance liquid chromatography （ UPLC ） was adopted in the test. Ofloxacin was used as the internal standard, and then the samples containing marbofloxacin were extracted from pork by trichloromethane. The collected samples were evaporated to dryness at 50 ℃. The extracted residues were reconstituted with mobile phase and cleaned by hexyl hydride. Chromatographic separation of marbofloxacin was performed on a Waters ACQUITY BEH RP18 2.1 mm × 50 mm,1.7 μm column using 0.2% trifluoroaceticacid （A） and acetonitrile （B） as the mobile phases （ 82：12 ）. The results showed that the calibration curve was good linear in the range of 10 to 1 000 μg/kg with the correlation coefficient of 0. 999 4. The limits of detection （LOD） were 5 μg/kg in pork tissue, and the limits of quantification （LOQ） were 10 μg/kg, respectively. The average recoveries varied from 85.80% to 103.20% at the three spiked levels of 50, 150 and 300 μg/kg. The intra - day relative standard deviation （RSD） and inter - day RSD were in the range of 2.1% to 3.8%, and 2.9% to 4.7%, respectively. The results indicate that this method is simple with high sensitivity, and can be used for the residue detection of related drugs.

关 键 词：超高效液相色谱(UPLC) 猪肉 麻保沙星 残留 检测 

分 类 号：S859.84[农业科学—临床兽医学] S879.2[农业科学—兽医学]