在考察了荧光胺、邻苯二甲醛、异硫氰酸荧光素和2，3-萘二醛等对磺胺类药物衍生效果的基础上，建立了采用改良 QuEChERS方法进行样品前处理，荧光胺在线柱后衍生，高效液相色谱-荧光检测法测定牛肉中16种磺胺残留量的方法。牛肉样品经1％（ v／v）乙酸乙腈溶液提取，改良 QuEChERS方法净化后取上清液进样，与荧光胺柱后在线衍生，荧光检测器检测。实验结果表明，16种磺胺类药物在0.024～2.533 mg／L 范围内线性关系良好，相关系数（ r）大于0.992，检出限为1.6～8.2μg／kg，平均加标回收率范围为66.6％～109.5％，相对标准偏差为0.9％～9.9％。该方法快速简便、灵敏度高、净化效果好，可用于牛肉中16种磺胺类药物的快速测定。
In this study,we investigated the effects of the four kinds of derivatization reagents, including fluorescamine,o-phthaladehyde,fluorescein isothiocyanate isomer and 2,3-naphtha-lenedicarboxaldehyde. A high performance liquid chromatography with fluorescence detection method for the rapid determination of 16 sulfonamide residues in beef was developed by using improved QuEChERS method for sample pretreatment and fluorescamine for online post-column derivatization. The beef samples were extracted with acetonitrile containing 1%( v/v ) acetic acid,cleaned-up by QuEChERS method,injected for online post-column derivatization with flu-orescamine,and then analysed with fluorescence detection. Under the optimized conditions of QuEChERS and chromatography,the 16 sulfonamide residues showed good linearities in the range of 0. 024-2. 533 mg/L with the correlation coefficients( r)higher than 0. 992. The limits of detection of the method were 1. 6 to 8. 2 μg/kg. The average recoveries of the 16 sulfonamide residues were in the range of 66. 6%-109. 5% with the relative standard deviations from 0. 9% to 9. 9%. The method has the advantages of rapidity,simplicity,high sensitivity and better purifi-cation effect. It is suitable for the rapid determination of the sulfonamide residues in beef.
参考文献
| [1] | Reig M;Toldra F.Veterinary drug residues in meat: concerns and rapid methods for detection.[J].Meat Science,20081/2(1/2):60-67. |
| [2] | Cai ZX;Zhang Y;Pan HF;Tie XW;Ren YP.Simultaneous determination of 24 sulfonamide residues in meat by ultra-performance liquid chromatography tandem mass spectrometry[J].Journal of chromatography, A: Including electrophoresis and other separation methods,20082(2):144-155. |
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