摘要
目的:建立一种同时测定丙烯酰氯及其杂质3-氯丙酰氯含量的高效液相色谱方法。方法:以苯胺作为衍生试剂柱前对丙烯酰氯进行衍生化处理,采用十八烷基硅烷键合硅胶柱,以0.1%磷酸水溶液和乙腈为流动相进行梯度洗脱。流速为1 mL/min;检测波长为254 nm;进样量为10μL;柱温为30℃。结果:样品检测中丙烯酰氯和3-氯丙酰氯的衍生色谱峰峰形良好且能达到基线分离,丙烯酰氯和3-氯丙酰氯分别在0.01~151.62μg/mL和0.02~2.95μg/mL范围内具有良好的线性关系(相关系数r>0.999),回收率范围分别是98.59%~99.77%和98.19%~99.54%(回收率RSD<1.0%)。结论:本研究建立的检测方法专属性强,检测灵敏度高,可用于丙烯酰氯的日常检测。
Objective:To establish a high performance liquid chromatography method for simultaneous determination of acryloyl chloride and the impurity 3-chloropropionyl chloride.Method:Anline was used as a derivatization reagent to derivatize acryloyl chloride.Seperation was carried out on an octadecylsilyl silica gel column.Gradient elution was performed with 0.1%phosphoric acid aqueous solution and acetonitrile as mobile phase.The flow rate was 1 mL/min.The detection wavelength was 254 nm.The injection volume was 10μL.The column temperature was 30℃.Results:The chromatographic derivations of acryloyl chloride and 3-chloropropionyl chloride showed good peak shape and achieved baseline seperation.The method established prestented good linearity from 0.01μg/mL to 151.62μg/mL for acryloyl chloride and from 0.02μg/mL to 2.95μg/mL for 3-chloropropionyl chloride with correlation coefficient greater than 0.999.The recovery range was from 98.59%to 99.77%for acryloyl chloride and from 98.19%to 99.54%for 3-chloropropionyl chloride with the relative standard deviation lower than 1.0%.Conclusion:The method established in the study shows strong specificity and high senstivity.It can be uesd for the daliy detection of acryloyl chloride.
作者
葛红娟
毛晓娜
吴岩
卜永海
何康永
唐祁匀
GE Hongjuan;MAO Xiaona;WU Yan;BU Yonghai;HE Kangyong;TANG Qiyun(Jiangsu Weiqida Pharmaceutical Co.,Ltd.,Nantong 226100,China)
出处
《山东化工》
2025年第12期125-127,共3页
Shandong Chemical Industry
关键词
丙烯酰氯
3-氯丙酰氯
衍生化
高效液相色谱
acryloyl chloride
3-chloropropionyl chloride
derivatization
high performance liquid chromatography
作者简介
并列第一作者:葛红娟,研究生,工程师,主要从事药物质量研究与开发工作;并列第一作者:毛晓娜,本科,工程师,主要从事药物质量研究与开发工作;通信作者:唐祁匀,本科,高级工程师,主要从事化学药物研发与产业化应用工作。
