HPLC and GC methods development for the analysis of key intermediate for synthesis of dicamba

doi:10.1016/j.cjche.2020.09.046

中国化学工程学报 ›› 2021, Vol. 33 ›› Issue (5): 112-117.DOI: 10.1016/j.cjche.2020.09.046

• Separation Science and Engineering • 上一篇下一篇

HPLC and GC methods development for the analysis of key intermediate for synthesis of dicamba

Zhenming Zhang^1,2, He Zhao³, Xiaohui Wang², Weiming Ni¹, Fengsheng Gao³, Jianrong Wang², Minjin Liu², Yongli Li¹

1 Key Laboratory of Power Station Energy Transfer Conversion and System, Ministry of Education, North China Electric Power University, Beijing 102206, China;
2 Jiangsu Changqing Agrochemical Co., Ltd., Yangzhou 225200, China;
3 Jiangsu Changqing Agrochemical Nantong Co., Ltd., Nantong 226000, China

收稿日期:2020-06-04 修回日期:2020-08-11 出版日期:2021-05-28 发布日期:2021-08-19
通讯作者: Yongli Li
基金资助:
This work was supported by National Key Research Development Program of China (2017YFB1103002, 2018YFB0604304), and National Natural Science Foundation of China (51821004).

HPLC and GC methods development for the analysis of key intermediate for synthesis of dicamba

Zhenming Zhang^1,2, He Zhao³, Xiaohui Wang², Weiming Ni¹, Fengsheng Gao³, Jianrong Wang², Minjin Liu², Yongli Li¹

1 Key Laboratory of Power Station Energy Transfer Conversion and System, Ministry of Education, North China Electric Power University, Beijing 102206, China;
2 Jiangsu Changqing Agrochemical Co., Ltd., Yangzhou 225200, China;
3 Jiangsu Changqing Agrochemical Nantong Co., Ltd., Nantong 226000, China

Received:2020-06-04 Revised:2020-08-11 Online:2021-05-28 Published:2021-08-19
Contact: Yongli Li
Supported by:
This work was supported by National Key Research Development Program of China (2017YFB1103002, 2018YFB0604304), and National Natural Science Foundation of China (51821004).

摘要/Abstract

摘要： The microreactor based hydroxylation process of 1,2,4-trichlorobezene for producing 2,5-dichlorphenol, the key intermediate of dicamba, is energy efficient and cost effective. But the 2,5-dicholorphneol is present in a mixed state after production. The reaction mixture contained the main by-product 2,4-dichlorophneol, low-content by-product 3,4-dichlorophneol, and other impurities. The difficulty in separation and analysis limits the application of this process widely. The current work aimed at establishing effective analysis methods by gas chromatography (GC) and high performance liquid chromatography (HPLC). The GC method was not able to separate 2,5-dichlorophenol and 2,4-dichlorophenol completely, but the developed HPLC method worked efficiently. The linear correlation coefficients of 2,5-dichlorophenol and 2,4-dichlorophenol were both higher than 0.999, and the average recovery was 100.33% for 2,5-dichlorophenol and 100.13% for 2,4-dichlorophenol, respectively. The relative standard deviations from precision tests were both less than 1%. The contents of 2,5-dichlorophenol and 2,4-dichlorophenol were determined with external standard method. The HPLC method has the advantages of simple operation, good separation efficiency, high accuracy and precision, and was successfully applied for both qualitative and quantitative analysis of 2,5-dichlorophenol and 2,4-dichlorophenol of the sample solution.

关键词: 2,5-dichlorophenol, 2,4-dichlorophenol, Chromatography, Separation, Chemical analysis

Abstract: The microreactor based hydroxylation process of 1,2,4-trichlorobezene for producing 2,5-dichlorphenol, the key intermediate of dicamba, is energy efficient and cost effective. But the 2,5-dicholorphneol is present in a mixed state after production. The reaction mixture contained the main by-product 2,4-dichlorophneol, low-content by-product 3,4-dichlorophneol, and other impurities. The difficulty in separation and analysis limits the application of this process widely. The current work aimed at establishing effective analysis methods by gas chromatography (GC) and high performance liquid chromatography (HPLC). The GC method was not able to separate 2,5-dichlorophenol and 2,4-dichlorophenol completely, but the developed HPLC method worked efficiently. The linear correlation coefficients of 2,5-dichlorophenol and 2,4-dichlorophenol were both higher than 0.999, and the average recovery was 100.33% for 2,5-dichlorophenol and 100.13% for 2,4-dichlorophenol, respectively. The relative standard deviations from precision tests were both less than 1%. The contents of 2,5-dichlorophenol and 2,4-dichlorophenol were determined with external standard method. The HPLC method has the advantages of simple operation, good separation efficiency, high accuracy and precision, and was successfully applied for both qualitative and quantitative analysis of 2,5-dichlorophenol and 2,4-dichlorophenol of the sample solution.

Key words: 2,5-dichlorophenol, 2,4-dichlorophenol, Chromatography, Separation, Chemical analysis

Zhenming Zhang, He Zhao, Xiaohui Wang, Weiming Ni, Fengsheng Gao, Jianrong Wang, Minjin Liu, Yongli Li. HPLC and GC methods development for the analysis of key intermediate for synthesis of dicamba[J]. 中国化学工程学报, 2021, 33(5): 112-117.

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HPLC and GC methods development for the analysis of key intermediate for synthesis of dicamba

HPLC and GC methods development for the analysis of key intermediate for synthesis of dicamba

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