饲料中磺胺氯吡嗪钠含量的高效液相色谱检测方法的建立

为建立饲料中磺胺氯吡嗪钠的高效液相色谱检测方法,饲料经乙腈提取,旋转蒸发浓缩,2 mL甲醇+8 mL 0.05mol.L-1KH2PO4溶解,固相萃取净化,0.2μm有机相滤器过滤后,回收液经Agilent 1100液相色谱仪进行检测。检测条件:在C18色谱柱上,流速为1.000 mL.min-1,柱温25℃,紫外检测波长为272 nm,流动相为乙腈和0.2%磷酸混合液(体积比为35∶65)。试验结果显示:磺胺氯吡嗪钠的色谱峰保留时间为7.5 min;在添加0.5、1和2μg.mL-1条件下,回收率为90.6%～97.1%;检测限为0.5 mg.kg-1,定量限为1.0 mg.kg-1,线性范围为0.50～10.00μg.mL-1,回归方程为Y=57.332X+2.972 9(R2=0.999 3);4种饲料样本的相对标准偏差(RSD)为1.0%～2.9%。结论:本试验所建立的高效液相色谱检测方法灵敏度高、准确性和重现性好,可以对饲料中的磺胺氯吡嗪钠进行定量检测。

Determination of sulfaclozine sodium in feed by high performance liquid chromatography

A high performance liquid chromatography(HPLC)method,a standard determination of sulfaclozine sodium in feeds,was established in this study,after extracted by acetonitrile,concentrated,dissolved with 2 mL methanol+8 mL 0.05 mol·L-1 KH2PO4 and cleaned by C18 SPE column,filtrated with 0.2 μm organic phase filter,then detected with Agilent 1100 liquid chromatography.The determination conditions were as follows:with C18 column,1.000 mL·min-1 of flow rate,25 ℃ of column temperature,UV detection wavelength under 272 nm,mobile phase by acetonitrile and 0.2% phosphoric acid volume ratio 35∶65.The results showed that the chromatographic peak retention time of sulfaclozine sodium chloride was 7.5 min.By the adding conditions of 0.5,1,2 μg·mL-1 of sulfaclozine sodium,the recovery rate was between 90.6%-97.1%.The limit of detection was 0.5 mg·kg-1.The limit of quantification was 1.0 mg·kg-1,the linear range was 0.50-10.00 μg·mL-1,Y=57.332X+2.972 9(R2=0.999 3),and the relative standard deviation(RSD)of four kinds of feed samples were 1.0%-2.9%.The results indicated that the HPLC method has a high sensitivity,good accuracy and precision,and it can be used for detecting residual feed sulfaclozine sodium effectively.