高效液相色谱法测定吡虫啉杀虫剂中4种关键杂质残留量  

HPLC Determination of 4 Key Impurities Residues in Imidacloprid Insecticide

作　　者：王根林[1] 孟颖 WANG Genlin;MENG Ying(Jiangsu Yangnong Chemical Group Co.,Ltd.,Yangzhou 225009,China)

机构地区：[1]江苏扬农化工集团有限公司,扬州225009

出　　处：《理化检验（化学分册）》2021年第6期533-536,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了高效液相色谱法同时测定吡虫啉杀虫剂中4种关键杂质硝酸胍、硝基胍、咪唑烷和2-氯-5-氯甲基吡啶的残留量的方法。样品2.000 g经20%(体积分数)甲醇溶液溶解后定容至100 mL。以Agilent Eclipse XDB C_(18)色谱柱(250 mm×4.6 mm,5μm)为固定相,以不同体积比的含有10 mmol·L^(-1)七氟丁酸的20 mmol·L^(-1)乙酸铵溶液和甲醇的混合液为流动相进行梯度洗脱,外标法定量。结果表明:4种关键杂质的质量浓度均在0.4~40 mg·L^(-1)内与其峰面积呈线性关系,检出限(3S/N)为0.13~0.15 mg·L^(-1)。按标准加入法进行回收试验,回收率为95.4%~103%,测定值的相对标准偏差(n=6)均小于2.0%。A method was proposed for the simultaneous determination of 4 key impurities,including guanidine nitrate,nitroguanidine,2-nitroaminoimidazoline and 2-chloro-5-chloromethylpyridine in imidacloprid insecticide by high performance liquid chromatography(HPLC).The sample of 2.000 g was dissolved in 20%(φ)methanol solution,and then made its volume up to 100 mL.The Agilent Eclipse XDB C_(18) chromatographic column(250 mm×4.6 mm,5μm)was used as stationary phase,and a mixture of 20 mmol·L^(-1) ammonium acetate solution with 10 mmol·L^(-1) heptafluorobutyric acid and methanol in different volume ratios was used as the mobile phase for gradient elution.External standard method was used for quantification.As shown by the results,linear relationships between values of peak area and mass concentration of 4 key impurities were found in the same range of 0.4-40 mg·L^(-1),with detection limits(3 S/N)ranging from 0.13 to 0.15 mg·L^(-1).Tests for recovery were made by standard addition method,giving results in the range of 95.4%-103%,and RSDs(n=6)of the determined values all less than 2.0%.

关 键 词：高效液相色谱法 吡虫啉 关键杂质 离子对试剂 

分 类 号：O657.7[理学—分析化学]