固相萃取-高效液相色谱法测定水中磺胺类药物  

HPLC Determination of Sulfonamides in Water with Solid-Phase Extraction

作　　者：隋丽丽[1] 隋崴崴[2] 江艳[1] 于岩[1] 

机构地区：[1]齐齐哈尔大学化学与化学工程学院,齐齐哈尔161006 [2]河北农业大学海洋学院,秦皇岛066003

出　　处：《理化检验（化学分册）》2013年第4期428-431,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：黑龙江省自然科学基金资助项目(B201101);齐齐哈尔大学青年教师科研启动计划项目(060033)

摘　　要：提出了固相萃取-高效液相色谱法测定水中3种磺胺类药物(磺胺甲噁唑、磺胺异噁唑和磺胺间甲氧嘧啶)的方法。水样经自制的阳离子交换固相萃取柱净化和富集后,以C18色谱柱(250mm×4.6mm,5μm)为固定相,以乙腈和2%(体积分数)乙酸溶液以体积比1比5的混合液为流动相进行分离,在波长270nm处用紫外检测器测定。3种磺胺类化合物的质量浓度均在0.005～0.5mg.L-1之间与其峰面积呈线性关系,方法检出限(3S/N)在2.4～3.7μg.L-1之间。方法用于水样中上述3种磺胺类化合物的测定,测定值的相对标准偏差(n=6)在2.6%～4.4%之间,加标回收率在88.6%～103%之间。SPE-HPLC was applied to the determinations of 3 sulfonamides in water, i. e. , sulfamethoxazole, sulfisoxazole and sulfamonomethoxine. The sulfonamides in sample were enriched on the self-made cation exchange SPE column, and separated on C18 column. A mixed solution of acetonitrile and 20/oo （9） acetic acid solution （mixed in the a ratio of 1 to 5） was used as mobile phase. UV-detection at 270 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 3 sulfonamides were kept in the same range of 0. 005-0. 5 mg·L^-1 , with detection limits （3S/N） in the range of 2.4-3. 7μg·L^-1. The proposed method was applied to the determination of the 3 sulfonamides in water sample, giving results of recovery obtained by standard addition method in the range from 88. 6% to 103% and RSD＇s （n=6） in the range of 2.6% to 4. 4%.

关 键 词：固相萃取 高效液相色谱法 磺胺类药物 

分 类 号：O652.63[理学—分析化学]