摘要
建立了同时测定牛奶中残留的9种磺胺类药物的固相萃取-高效液相色谱分析方法。牛奶样品经磷酸盐缓冲液稀释后高速离心去除脂肪,过C18小柱,用水淋洗,甲醇洗脱,洗脱液经氮气吹干后用乙酸乙酯溶解,并过氨基固相萃取小柱净化,用正己烷及水淋洗,以甲醇-乙腈-水(含1%乙酸)(体积比为1:1:8)洗脱,洗脱液用于高效液相色谱分析。采用InertsilODS-3C18柱分离,以水-乙酸和甲醇-乙腈为流动相进行梯度洗脱,二极管阵列检测器检测,外标法定量。9种磺胺类药物标准曲线的线性回归系数均在0.9999以上,线性范围为25～5000μg/L,检出限为1.7～2.8μg/L,定量限为5.7～9.2μg/L。在10,20,40μg/L添加水平下的添加回收率为72.1%～88.3%,相对标准偏差为2.3%～5.0%。该方法具有快速、灵敏的特点,符合现行兽药残留分析的要求。
A simple, rapid, sensitive and reliable high performance liquid chromatographic method for the simultaneous determination of nine sulfonamides （SAs） （ sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxypyridazine, sufamonomethoxine, sulfachloropyridazine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline） in milk was developed. The method includes the shaking of the milk with phosphate buffer, centrifugation, and cleaning up on a C18 solid-phase extraction cartridge. The C18 cartridge was washed with water, and the SAs were eluted with methanol. After the evaporation, the residue was dissolved in ethyl acetate, and cleaned up on an amino solid-phase extraction column. Analytical separation was performed on an Inertsil ODS-3 column with photodiode-array detection at 270 nm under the gradient condition. The mean recoveries of SAs at the spiked levels of 10, 20, 40 μg/L were between 72. 1% and 88.3%. The relative standard deviations were between 2.3% and 5.0%. The detection limits were 1.7 - 2. 8 μg/L, and the quantification limits wer 5.7 - 9.2 μg/L.
出处
《色谱》
CAS
CSCD
北大核心
2007年第5期728-731,共4页
Chinese Journal of Chromatography
关键词
高效液相色谱法
固相萃取
磺胺类药物
残留分析
牛奶
high performance liquid chromatography （HPLC）
solid phase extraction （ SPE ）
sulfonamides
residue analysis
milk
