HPLC法检测对氯苯甲酰氯中位置异构体杂质

摘要

目的：建立高效液相色谱法（ HPLC ）测定对氯苯甲酰氯中位置异构体杂质邻氯苯甲酰氯、间氯苯甲酰氯的方法。方法：对氯苯甲酰氯样品加水完全水解后，在色谱条件为SUPELCO Discovery C-18（250 mm ×4.6 mm，5μm）色谱柱，以乙腈和水（磷酸调pH至2.5）为流动相，梯度洗脱，流速为1 mL· min－1，检测波长为230 nm，柱温为25℃，进样量为10μL的条件下进行检测。结果：邻氯苯甲酰氯、对氯苯甲酰氯摩尔浓度在1.55～9.31×10－6 mol· L－1范围内线性关系良好，线性回归方程为Y邻＝4.6977X－0.3132（r＝0.9991），Y间＝6.0618X ＋0.9108（r＝0.9992）；邻氯苯甲酰氯、对氯苯甲酰氯检出限分别为1.14×10－7 mol· L－1、0.74×10－7 mol· L－1，平均加标回收率分别为95.8％、98.7％，RSD分别为1.23％、1.86％。结论：本方法简单、灵敏，重现性好，准确度高，可用于对氯苯甲酰氯中位置异构体杂质的控制。%Objective:HPLC method has been developed for sensitive determination of 2-chlorobenzoyl chloride and 3-chlorobenzoyl chloride ( position isomers) in parachlorobenzoyl chloride.Methods: After adding water complete hydrolysis of parachlorobenzoyl chlo-ride samples, 2-chlorobenzoyl chloride and 3-chlorobenzoyl chloride were separated and analyzed on a SUPELCO Discovery C-18 column (250 mm ×4.6 mm,5μm) with acetonitrile /phosphoric acid water solution (pH=2.5) as the mobile phase at a flow rate of 1.0 mL · min-1 , the detection wavelength was 230nm and the column temperature was 25 ℃.Results:The results showed that the linear ranges were from 1.55 to 9.31 ×10 -6 mol· L-1 for 2-chlorobenzoyl chloride and 3-chlorobenzoyl chloride by the external standard method.The linear regression equations were Y2 =4.6977X-0.3132(r=0.9991),Y3 =6.0618X+0.9108(r=0.9992),respectively.The detection limits of 2-chlorobenzoyl chloride and 3-chlorobenzoyl chloride were 1.14 ×10 -7 mol· L-1 and 0.74 ×10-7 mol· L-1 ,respectively.The average recoveries of 2-chlorobenzoyl chloride and 3-chlorobenzoyl chloride were 95.8% and 98.7% with the relative standard devia-tions of 1.23%and 1.86%,respectively.Conclusion:The method is accurate,reliable,sensitive,simple and suitable for the determina-tion of position isomers in parachlorobenzoyl chloride.