丙烯酰氯及其杂质3-氯丙酰氯的含量测定

　　

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1mL/min；检测波长为254nm；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。

关键词：丙烯酰氯；3-氯丙酰氯；衍生化；高效液相色谱

Determination of acryloyl chloride and the impurity 3-chloropropionyl chloride

Ge Hongjuan, Tang Qiyun^*

(Jiangsu Weiqida pharmaceutical Co., Ltd, Jiangsu Nantong 226100)

Abstract: 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 1mL/min. The detection wavelength was 254nm. 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.

Key words: acryloyl chloride; 3-chloropropionyl chloride; derivatization; high performance liquid chromatography

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