第 52 卷第 4 期 Vol. 52 No. 4 2022 年 8 月 Aug 2022

所属栏目：分析与测试 气相色谱法同时测定环磷酰胺中间体3-氨基丙醇的四种有关物质

王 艳1，周思源1，徐 静1，刘 志2，程青芳1* （1.江苏海洋大学 药学院，江苏 连云港 222005；2. 连云港贵科药业有限公司，江苏 连云港 222000）

摘　要：建立了环磷酰胺中间体3-氨基丙醇中四种有关物质1-氨基-2-丙醇、2-氨基-1-丙醇、N-甲基-2-吡咯烷酮和3-羟基丙腈的气相色谱同时检测方法。采用TG-WAXMS B 毛细管色谱柱对3-氨基丙醇中这四种有关物质进行分离。结果显示，四种有关物质在所测浓度范围内线性关系良好（R2>0.99），定量限≤7.999 μg/mL，检测限≤2.400 μg/mL。平均加标回收率为89.2%~116.6%，RSD≤6.3%（n=9），且对照品溶液和供试品溶液在25 ℃放置24 h稳定，RSD≤3.8%（n=7）。将所建的方法应用于检测3批3-氨基丙醇样品，其中，1-氨基-2-丙醇、N-甲基-2-吡咯烷酮和3-羟基丙腈均未检出，检出2-氨基-1-丙醇的含量为0.01%~0.02%。所建立的分析方法灵敏度高、专属性和准确度好，适用于同时测定环磷酰胺中间体3-氨基丙醇中的这四种有关物质。

关键词：气相色谱法；环磷酰胺中间体；3-氨基丙醇；有关物质；方法学验证

中图分类号：R917　　文献标识码：A　　文章编号：1009-9212（2022）04-0079-05

Simultaneous Determination of Four Related Substances in Cyclophosphamide Intermediate 3-Amino-propanol by GC

WANG Yan1, ZHOU Si-yuan1, XU Jing1, LIU Zhi2, CHENG Qing-fang1* (1.School of Pharmacy, Jiangsu Ocean University, Lianyungang 222005, China; 2. Lianyungang Guike Pharmaceutical Co., Ltd., Lianyungang 222000, China)

Abstract：A GC method was established for the determination of related substances 1-amino-2-propanol, 2-amino-1-propanol, N-methyl-2-pyrrolidone and 3-hydroxypropanitrile in cyclophosphamide intermediate 3-amino-propanol. The separation of this four related substances was performed in a TG-WAXMS B capillary column. The results showed that the linearities of the four related substances in the test concentration ranges were good. The quantification limits of the four related substances were less than or equal to 7.999 μg/mL. Their detection limits were less than or equal to 2.400 μg/mL. The average recoveries of 1-amino-2-propanol, 2-amino-1-propanol, N-methyl-2-pyrrolidone and 3-hydroxypropanitrile were 89.2%~116.6% with RSD≤6.3%(n=9). The reference solution and test solution were stable for at least 24 h at 25 ℃ with RSD≤3.8%(n=7). This proposed method was applied to detect three 3-amino-propanol samples, and 1-amino-2-propanol, N-methyl-2-pyrrolidone and 3-hydroxypropanitrile were not detected, but the detection range of 2-amino-1-propanol was 0.01%~0.02%. With high sensitivity, good specificity and accuracy, the method established in this work is suitable for the simultaneous determination of the four related substance in cyclophosphamide intermediate 3-amino-propanol.

Key words：GC; cyclophosphamide intermediate; 3-amino-propanol; related substances; methodological verification

作者简介：王 艳（1994—），女，江苏宿迁人，硕士研究生，研究方向：药物分析（E-mail：1661222855@qq.com）。

联 系 人：程青芳，教授，研究方向：药物合成和药物质量控制（E-mail：489417058@qq.com）。

收稿日期：2021-11-17