固相萃取–高效液相色谱法测定蔬菜中8种磺胺类抗生素

建立固相萃取–高效液相色谱同时测定蔬菜中8种磺胺类抗生素(SAs)的分析方法。蔬菜样品经10 m L乙腈(添加2 g Na_2SO_4+0.1 g CH_3COONa+0.1 g Na_2EDTA)超声提取,提取液用正己烷液–液萃取去脂,经C18–OH固相萃取小柱净化后用高效液相色谱法紫外检测器测定。检测波长为270 nm,柱温为25℃,以乙腈–0.01 mol/L磷酸水溶液为流动相,采用梯度洗脱程序,8种SAs可以较好分离,质量浓度在0.10~100.00 mg/L范围内与色谱峰面积均成良好的线性关系,相关系数为0.999 7~0.999 9,方法检出限为25~75μg/kg,定量限为54~140μg/kg。8种SAs的加标平均回收率为68.70%~122.7%,测定结果的相对标准偏差为1.8%~4.5%(n=5)。该法具有灵敏度高、样品处理简单等优点,可用于蔬菜中磺胺类抗生素的检测。

Determination of Eight Kinds of Sulfonamide Antibiotics in Vegetable by Solidphase Extraction-High Performance Liquid Chromatography

A method for determining eight sulfonamides antibiotics residue in vegetable samples by solid phase extraction-high performance liquid chromatography was established. The vegetable samples were ultrasonically extracted with acetonitrile (adding 2 g anhydrous sodium sulfate, 0.1 g sodium acetate and 0.1 g disodium ethylenediamine tetraacetate) and the extracted solution was extracted with n-hexane, cleaned by C18-OH SPE cartridge, then detected by using HPLC-UV. The detection wavelength was 270 nm and the column temperature was 25℃ . Acetonitrile-0.01 mol/L phosphoric acid solution was used as gradient elution for separation, and better separation of eight kinds of sulfonamides was achieved. The concentration of sulfonamide was linear with its chromatographic peak area in the range of 0.10-100.00 mg/L with the correlation coefficients of 0.9997-0.9999. The detection limits (S/N=3) of the method were 25-75 μg/kg and the quantification limits (S/N=10) were 54-140 μg/kg. The average recovery rates of eight kinds of sulfonamides were 68.70%-122.7% and the relative standard deviations of detection results were 1.8%-4.5%(n=5). The method has the advantages of high sensitive, simple pretreatment, it is suitable for the detection of sulfonamide antibiotics in vegetables.