第 51 卷第 5 期Vol. 51 No. 5
2021 年 10 月Oct 2021
所属栏目：分析与测试

硝基联苯、氨基联苯及啶酰菌胺的高效液相色谱分析方法
高 翀1，陆亚军1，庞怀林2 （1. 上海泰禾化工有限公司，上海201612；2. 南通泰禾化工股份有限公司，江苏 南通 226407）
摘　要：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.×5 μm）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1.000 0，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1.000 0，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1.000 0，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。
关键词：啶酰菌胺；4-氯-2'-硝基联苯；4-氯-2'-氨基联苯；高效液相色谱
中图分类号：O657.7+2　　文献标识码：A　　文章编号：1009-9212（2021）05-0096-06
HPLC Analysis of Nitrobiphenyl, Aminobphenyl and Boscalid
GAO Chong1, LU Ya-Jun1, PANG Huai-lin2 (1. CAC Shanghai Chemicals Co., Ltd., Shanghai 201612, China; 2. CAC Nantong Chemicals Co., Ltd., Nantong 226407, China)
Abstract：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.×5 μm) 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 1.000 0; 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 1.000 0; 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.
Key words：Boscalid; 4-chloro-2'-nitrobiphenyl; 4-chloro-2'-amino biphenyl; HPLC
作者简介：高 翀（1985—），男，上海人，研究方向：农药及精细化工分析（E-mail：chong_gao@cacch.com）。
收稿日期：2021-08-03