Determination of sulfaclozine sodium in feed by high performance liquid chromatography | 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

Chinese. 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。

English. 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-L 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 0.50-10.00μg・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.