试样中残留磺胺药物用乙腈提取并经正己烷萃取和通过碱性氧化铝层析柱进行净化.所得乙腈-水(30+70)洗脱液用于高效液相色谱法测定.采用C18色谱柱(250 mm×4.6 mm)作固定相,以乙腈(A)及乙腈+乙酸+水(20+1+79)的混合液(B)按不同比例混合液作流动相进行梯度淋洗使5种磺胺药物分离,最后在270 nm波长处作紫外检测,所测定的磺胺药物的质量浓度与其峰面积之间在0.05~1.00 mg·L-1范围内呈线性关系.方法的测定下限(S/N=10)为0.04 mg·kg-1,以猪肉样品为基体加入3种药物的标准溶液进行回收试验,测得回收率在73.65%~93.45%之间.

Residual amounts of sulfanilamide drugs in the sample were extracted with acetonitrile,and purified by extraction with n-hexane and adsorption on chromatographic column packed with basic aluminum oxide.Sulfanilamides in the eluate (acetonitrile and water mixed in the ratio of 3+7) were separated and determined by HPLC.A C18 column (250 mm×4.6 mm) was used as stationary phase,and mixed solutions of acetonitrile (A) and mixture of acetonitrile+acetic acid+water (20+1+79) (B) in different ratio were used as mobile phase in the gradient elution.UV-detections at 270 nm were used in the determinations.Linear relationship between values of peak area and mass concentration of the drugs was kept in the range of 0.05-1.00 mg·L-1.Limit of determination of the method was found to be 0.04 mg·kg-1.On the base of a meat sample,test for recovery was made by addition of standard solutions of 3 drugs,and values of recovery found were in the range of 73.65%-93.45%.