高效液相色谱法同时测定大豆中10种磺酰脲类除草剂的残留量

首次建立了同时检测大豆中10种磺酰脲类除草剂(环氧嘧磺隆、噻吩磺隆、甲磺隆、醚苯磺隆、氯磺隆、苄嘧磺隆、氟磺隆、吡嘧磺隆、氯嘧磺隆和氟嘧磺隆)多残留量的反相高效液相色谱(RP-HPLC)方法。样品经乙腈提取、正己烷液-液分配、Florisil填充柱净化后,采用RP-HPLC-二极管阵列检测器检测(DAD)法测定,外标法定量。对样品前处理和色谱分离条件进行了详细的研究和优化。10种磺酰脲类除草剂的质量浓度在0.1~10.0 mg/L范围内其浓度与峰面积的线性关系良好,相关系数为0.9996~0.9997;在

Simultaneous Determination of Ten Sulfonylurea Herbicide Residues in Soybeans by High Performance Liquid Chromatography

A reversed-phase high performance liquid chromatographic (RP-HPLC) method has been developed for the simultaneous determination of ten sulfonylurea herbicide (oxasulfuron, thifensulfuron-methyl, metsulfuron-methyl, triasulfuron, chlorsulfuron, bensulfuron-methyl, prosulfuron, pyrazosulfuron-methyl, chlorimuron-ethyl and primisufuron-methyl) residues in soybeans. Sulfonylurea herbicides were extracted with acetonitrile, followed by hexane partitioning. After the extract was cleaned up with a Florisil column, sulfonylurea herbicides were analyzed by HPLC-photo diode array detector (DAD) and quantified by external standard method. The pre-treatment method of the samples and the chromatographic conditions of the analysis were critically examined. The linear ranges of 10 sulfonylureas were 0.1 - 10.0 mg/L, and the correlation coefficients were 0.999 6 - 0.999 7. The average recoveries of ten sulfonylurea herbicides in spiked soybeans ranged from 69.8% to 100.7%, and the relative standard deviations were between 1.89% and 10.43%. The limit of detection was 20 microg/kg. The results have indicated that the method developed is easier, faster, and has better purification effect. It has also demonstrated that this multiresidue analytical method can meet the requirements for the simultaneous determination of many sulfonylurea herbicides in import and export inspection for soybeans.