硝基联苯、氨基联苯及啶酰菌胺的高效液相色谱分析方法

HPLC Analysis of Nitrobiphenyl,Aminobphenyl and Boscalid

建立了一种高效液相色谱定量方法,测定以4-氯-2'-硝基联苯制备4-氯-2'-氨基联苯合成啶酰菌胺路线各步反应中的有效成分含量。采用InertSustain ODS-C18不锈钢柱(250 mm×4.6 mm i.d.×5μm)和二极管阵列检测器,以乙腈和0.02%磷酸水为流动相,流速为1.0 mL/min,在220 nm波长下对中间体4-氯-2'-硝基联苯进行分离和定量分析;在254 nm波长下对中间体4-氯-2'-氨基联苯进行分离和定量分析;在254 nm波长下对啶酰菌胺进行分离和定量。分析结果表明,4-氯-2'-硝基联苯保留时间约24.3 min,线性相关系数为1.0000,标准偏差为0.04,变异系数为0.34%,平均回收率为100.04%;4-氯-2'-氨基联苯保留时间约18.0 min,线性相关系数为1.0000,标准偏差为0.05,变异系数为0.33%,平均回收率为99.94%;啶酰菌胺保留时间约11.9 min,线性相关系数为1.0000,标准偏差为0.21,变异系数为0.32%,平均回收率为100.09%。方法操作简便,精密度与准确度较高,满足定量分析要求。

A HPLC method was established for determination of active ingredients in each reaction step of the synthetic route in which 4-chloro-2'-amino biphenyl was prepared from 4-chloro-2'-nitrobiphenyl and used to synthesize Boscalid.The sample was separated and analyzed using Eclipse ODS-C18 stainless steel column(250 mm×4.6 mm i.d.×5μm)equipped with UV detector at 220 nm for 4-chloro-2'-nitrobiphenyl,while a wavelength of 254 nm was set for the determination of 4-chloro-2'-amino biphenyl and Boscalid.A mixture of acetonitrile and 0.02%phosphoric acid solution was used as the mobile phase with a flow rate of 1.0 mL/min.Results showed the fpllowings:the retention time(RT)of 4-chloro-2'-nitrobiphenyl was 24.3 min;the linear correlation coefficient(R2)was 1.0000;the standard deviation(SD)was 0.04;the variation coefficient(CV)was 0.34%;and average recovery was 100.04%;the RT of 4-chloro-2'-amino biphenyl was 18.0 min with a R2 of 1.0000,SD of 0.05;CV was of 0.33%;and average recovery was 99.94%.The RT of Boscalid was of 11.9 min,while the R2 was 1.0000;SD was of 0.21;CV was of 0.32%;and average recovery of 100.09%.This method is of high accuracy,short time,and convenience.