UPLC-MS/MS法测定水产品中7种喹诺酮类兽药残留  

UPLC-MS/MS for the Determination of seven Quinolones Residues in Aquatic Products Drug

作　　者：陶威 张苏珍 田蕴 王益军 龚其龙 彭程 TAO Wei;ZHANG Suzhen;TIAN Yun;WANG Yijun;GONG Qilong;PENG Cheng(Lian Yun Gang Animal Products Inspection Center,Lianyungang,Jiangsu 222000,China;Lian Yun Fishery Technology Extension Station,Lianyungang,Jiangsu 222042,China;Jurong District Fisheries Technology Promotion Station,Zhenjiang,Jiangsu 212400,China)

机构地区：[1]连云港市畜产品质量监督检验测试中心,江苏连云港222000 [2]连云港市连云区渔业技术推广站,江苏连云港222042 [3]句容市水产技术指导站,江苏镇江212400

出　　处：《水产养殖》2023年第3期26-32,52,共8页Journal of Aquaculture

基　　金：2021年农产品质量安全监测项目(苏农质[2021]1号)。

摘　　要：采用超高效液相色谱-串联质谱(UPLC-MS/MS)法,检测水产品中7种喹诺酮药物残留。选取青鱼、泥鳅和南美白对虾样品,用1%甲酸-乙腈超声提取后,经Oasis?Prime HLB固相萃取柱一步净化,氮吹浓缩,最后用10%甲醇复溶,0.1%甲酸水和纯甲醇作为流动相进行梯度洗脱,流量为0.3 mL/min,在电喷雾-多反应监测正离子模式下,7种喹诺酮(QNs)均采用内标法定量。结果表明,7种QNs药物在1.0~100.0μg/kg范围内,呈良好的线性关系,相关系数(R2)均高于0.998000。7种QNs在空白样品中添加浓度分别为5.0,1.0和20.0μg/kg时,在青鱼中回收率为92.71%~105.31%,泥鳅中回收率为92.31%~109.38%,南美白对虾中回收率为92.31%~106.76%。该方法具有较好的准确度和重复性。按照特征离子色谱峰信噪比(S/N)=3计算得出,7种QNs检出限为0.01~0.34μg/kg,定量限为0.04~0.87μg/kg。指出,该方法操作简便,灵敏度高,准确度好,适合大批量水产品中7种喹诺酮药物残留的检测分析。Ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was used to detect seven quinolone(QNs)residues in aquatic products.This study used Mylopharyngodon piceus,Misgurnus anguillicaudatus and Penaeus vanamei as experimental animals.Samples was ultrasonically extracted with 1%formic acid-acetonitrile,purified by Oasis B Prime HLB cartridge,Nitrogen blow enrichment 0.1%formic acid water and pure methanol were used as mobile phases,the flow rate was 0.3 mL/min,and electrospray-multi-re-action monitoring positive ion mode monitoring.All 7 QNs were quantified by internal standard method.The re-sults showed that 7 QNs drugs had a good linear relationship of 1.0 to 100.0μgkg and the correlation cofficient(R)was higher than 0.998000.When the concentrations of 7 QNs were 5.0,10.0 and 20.0μugkg in blank sam-ples,the recoveries were 92.71%-105.31%in M.piceus,92.31%-109.38%in M.angullicaudatus and 92.31%-106.76%in P.vannamei.The results show that the method has good accuracy and repeatability.According to the characteristic ion chromatographic peak signal-to--noise ratio(S/N)=3,the detection limits of 7 QNs were 0.01-0.34μg/kg,and the quantitative limits were 0.04-0.87μgkg.The method is simple,sensitive and accurate.It is suitable for the detection and analysis of 7 QNs in large quantities of aquatic products.

关 键 词：水产品 喹诺酮 药物残留 超高效液相色谱-串联质谱 

分 类 号：O657.72[理学—分析化学]