固相萃取-高效液相色谱法同时测定水产品中15种磺胺类药物残留

Simultaneous Determination of 15 Sulfonamides Residues in Aquatic Products by Solid Phase Extraction-High Performance Liquid Chromatography

摘要:

建立固相萃取-高效液相色谱法(solid phase extraction-high performance liquid chromatography, SPE-HPLC)同时检测水产品中15种磺胺类药物(sulfonamides，SAs)残留。样品用乙酸乙酯提取，正己烷脱脂，PCX(polymer cation exchange)固相萃取柱净化，采用高效液相色谱法检测，色谱条件为：Waters C₁₈ (4.6 mm×250 mm，5.0 μm)色谱柱分离，以甲醇和含体积分数1.1%乙酸的PBS缓冲液(0.01 mol/L)为流动相进行梯度洗脱，检测波长为270 nm。15种SAs在65 min内达到完全分离，在0.5~10.0 μg/mL时线性关系良好，相关系数均大于0.990 0；方法检出限为10~20 μg/kg，定量限为20~60 μg/kg；对空白鱼肉样品进行了3个质量分数水平(500、 1 000、 2 000 μg/kg)的加标实验，测定其空白加标回收率为73.1%~109.6%，相对标准偏差(relative standard deviations，RSDs) 在1.0%~6.7%。实验建立的检测方法重现性和稳定性好、检出限低。对江西10个不同品种的水产品中磺胺类药物残留进行了采样检测，结果均未检出，表明江西水产品中磺胺类药物残留情况并不严重。

Abstract:

A method of simultaneous determination of 15 sulfonamides residues in aquatic products was established by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted with ethyl acetate, degreased with n-hexane, and purified by polymer cation exchange (PCX) solid phase extraction column. The analysis was performed by high performance liquid chromatography with a chromatographic condition of separation on a Waters C₁₈ column (4.6 mm×250 mm, 5.0 μm) under gradient elution mode with methanol and PBS solution containing 1.1% acetic acid (0.01 mol/L) as the mobile phase. The target analytes were detected at the wavelength of 270 nm. The 15 sulfonamides were completely separated within 65 min, showing a good linear relationship within 0.5~10.0 μg/mL with correlation coefficients greater than 0.990 0. The limits of detection were in the range of 10~20 μg/kg, and the limits of quantitation were 20~60 μg/kg. The blank recovery rates of spiked samples at three mass fraction levels (500, 1 000, 2 000 μg/kg) ranged from 73.1% to 109.6% with the relative standard deviations (RSDs) of 1.0%~6.7%. The established detection method in this study showed good reproducibility, stability, and low detection limit. The residues of SAs in 10 different species of aquatic products from Jiangxi province were sampled and detected, and no residues were detected, indicating that the residues of SAs in aquatic products from Jiangxi province were not severe.