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

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.