水产品中螺旋霉素、替米考星、泰乐菌素与北里霉素残留量的超高效液相色谱-紫外检测法同时测定  

Simultaneous Determination of Spiramycin,Tilmicosin,Tylosin and Kitasamycin Residues in Fishery Products by UPLC-TUV Method

作　　者：刘永涛[1,2] 艾晓辉[1,2] 邹世平[1,2] 杨红[1,2] 

机构地区：[1]中国水产科学研究院淡水渔业研究中心,江苏无锡214081 [2]中国水产科学研究院长江水产研究所农业部淡水鱼类种质监督检验测试中心,湖北荆州434000

出　　处：《分析测试学报》2010年第3期316-320,共5页Journal of Instrumental Analysis

基　　金：中央级公益性科研院所基本科研业务费专项资金资助项目

摘　　要：建立了水产品肌肉组织中螺旋霉素、替米考星、泰乐菌素、北里霉素同时测定的超高效液相色谱-紫外检测（UPLC—TUV）方法。样品经乙腈提取后，浓缩至近干，用4％NaCl溶解残渣，正己烷除脂，经固相萃取小柱净化，乙腈洗脱；以乙腈-25mmol／L磷酸二氢铵（pH2．5，含10％乙腈）为流动相，以ACQUITYUPLCBEHC18为分离柱，柱温为45℃，流速为0．3mL／min，紫外检测。方法在0．100—20．0mg／L范围内呈线性相关，螺旋霉素、替米考星、泰乐菌素和北里霉素的相关系数分别为0．9987、0．9993、0．9994和0．9980。平均回收率为70％～102％，相对标准偏差为2．9％-11．2％，螺旋霉素、替米考星、泰乐菌素和北里霉素的检出限分别为25、25、50、75μg／kg。方法满足水产品肌肉组织中螺旋霉素、替米考星、泰乐菌素和北里霉素的残留量测定。An ultra high performance liquid chromatographic （UPLC） method for simultaneous determination of residues of spiramycin （ SPM ）, tilmicosin （ TIL）, tylosin （TYL） and kitasamycin （KIT） in fishery products has been developed. The muscle tissue sample was extracted by acetonitrile, and the extracts were evaporated to near dryness and redissolved in 4% NaCl water solution. The extracts were defatted with hexane, and cleaned up on a HLB SPE column. The analytes was separated on ACQUITY UPLC BEH C18with acetonitrile -25 mmoL/L NH4H2PO4 solution （pH 2. 5, containing 10% acetonitrile） as mobile phase at flow rate of 0.3 mL/min and column temperature of 45℃. The TUV detector was set at the mode of wavelength events. The external standard was used for quantitation analysis. The standard curves were linear in the range of 0. 100 -20. 0 mg/L for all analytes with correlation coefficients of 0. 998 0 -0. 999 4. The detection limits for spiramycin, tilmicosin, tylosin and kitasamycin were 25, 25, 50, 75 μg/kg, respectively. The average recoveries of four analytes at spiking levels of 0. 10 - 1.0 mg/kg ranged from 70% to 102%. The relative standard deviations were between 2. 9% and 11.2%. The method could meet the requirement for simultaneously determi- nation of spiramycin, tilmicosin, tylosin and kitasamycin residues in fishery products muscle sampies.

关 键 词：水产品 螺旋霉素 替米考星 泰乐菌素 北里霉素 残留量 超高效液相色谱 

分 类 号：O657.72[理学—分析化学] S859.79[理学—化学]