| 第 52 卷第 4 期 |  | Vol. 52 No. 4 | | 2022 年 8 月 | Aug 2022 |
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所屬欄目：分析與測試
氣相色譜法同時(shí)測定環(huán)磷酰胺中間體3-氨基丙醇的四種有關(guān)物質(zhì) |
| 王 艷1，周思源1，徐 靜1，劉 志2，程青芳1*
（1.江蘇海洋大學(xué) 藥學(xué)院，江蘇 連云港 222005；2. 連云港貴科藥業(yè)有限公司，江蘇 連云港 222000） |
| 摘 要：建立了環(huán)磷酰胺中間體3-氨基丙醇中四種有關(guān)物質(zhì)1-氨基-2-丙醇、2-氨基-1-丙醇、N-甲基-2-吡咯烷酮和3-羥基丙腈的氣相色譜同時(shí)檢測方法。采用TG-WAXMS B 毛細管色譜柱對3-氨基丙醇中這四種有關(guān)物質(zhì)進(jìn)行分離。結果顯示，四種有關(guān)物質(zhì)在所測濃度范圍內線(xiàn)性關(guān)系良好（R2>0.99），定量限≤7.999 μg/mL，檢測限≤2.400 μg/mL。平均加標回收率為89.2%~116.6%，RSD≤6.3%（n=9），且對照品溶液和供試品溶液在25 ℃放置24 h穩定，RSD≤3.8%（n=7）。將所建的方法應用于檢測3批3-氨基丙醇樣品，其中，1-氨基-2-丙醇、N-甲基-2-吡咯烷酮和3-羥基丙腈均未檢出，檢出2-氨基-1-丙醇的含量為0.01%~0.02%。所建立的分析方法靈敏度高、專(zhuān)屬性和準確度好，適用于同時(shí)測定環(huán)磷酰胺中間體3-氨基丙醇中的這四種有關(guān)物質(zhì)。 |
| 關(guān)鍵詞：氣相色譜法；環(huán)磷酰胺中間體；3-氨基丙醇；有關(guān)物質(zhì)；方法學(xué)驗證 |
| 中圖分類(lèi)號：R917 文獻標識碼：A 文章編號：1009-9212（2022）04-0079-05 |
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| 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 |
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作者簡(jiǎn)介：王 艷（1994—），女，江蘇宿遷人，碩士研究生，研究方向：藥物分析（E-mail：1661222855@qq.com）。
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聯(lián) 系 人：程青芳，教授，研究方向：藥物合成和藥物質(zhì)量控制（E-mail：489417058@qq.com）。
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收稿日期：2021-11-17
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