| 第 52 卷第 2 期 |  | Vol. 52 No. 2 | | 2022 年 4 月 | Apr 2022 |
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所屬欄目：分析與測試
GC-MS測定磷酸西格列汀中基因毒性雜質(zhì)水合肼 |
| 李善金1，徐 盼1，楊漢躍2，程青芳1*
（1. 江蘇海洋大學(xué) 藥學(xué)院，江蘇 連云港 222005；2.江蘇德源藥業(yè)股份有限公司，江蘇 連云港 222047） |
| 摘 要：建立了GC-MS測定磷酸西格列汀中基因毒性雜質(zhì)水合肼含量的檢測方法。采用DB-1701（14%-氰丙基-苯基）甲基聚硅氧烷毛細管柱進(jìn)行檢測，醋酸中通過(guò)丙酮衍生化處理，在全掃描模式下確定水合肼衍生物的定量離子m/z 為97。結果顯示，水合肼衍生物在10.36~230.25 ng/mL濃度范圍內線(xiàn)性關(guān)系良好，相關(guān)系數r=0.999 1；水合肼衍生物的定量限、檢測限分別為10.4、3.1 ng/mL。平均加標回收率為102%~112%，RSD≤3%（n=12），系統適用性溶液25 ℃放置24 h內穩定，RSD≤6%，上述方法用于檢測3批磷酸西格列汀樣品，均未檢出水合肼衍生物。所建立分析方法靈敏度高、專(zhuān)屬性強，適用于磷酸西格列汀中基因毒性雜質(zhì)水合肼的測定。 |
| 關(guān)鍵詞：磷酸西格列��；GC-MS；基因毒性雜質(zhì)；水合肼；衍生化 |
| 中圖分類(lèi)號：TQ460.7 文獻標識碼：A 文章編號：1009-9212（2022）02-0064-05 |
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| Determination of Genotoxic Impurity Hydrazine Hydrate in Sitagliptin Phosphate by GC-MS |
| LI Shan-jin1, XU Pan1, YANG Han-yue2, CHENG Qing-fang1*
(1. School of Pharmacy, Jiangsu Ocean University, Lianyungang 222005, China; 2. Jiangsu Deyuan Pharmaceutical Co., Ltd., Lianyungang 222047, China) |
| Abstract：A GC-MS method was established for the determination of the genotoxic impurity hydrazine hydrate in Sitagliptin Phosphate. The detection was performed on DB-1701 (14%-cyanopropyl-phenyl) methyl polysiloxane capillary column. The quantitative ion m/z 97 was scanned in the full scanning mode by derivatization using acetone and glacial acetic acid. The results showed that the hydrazine hydrate derivative in a test concentration range between 10.36 ng/mL to 230.25 ng/mL had good linear relationship (r=0.999 1). The quantification and detection limits of the hydrazine hydrate derivative were 10.4 ng/mL and 3.1 ng/mL respectively. The average recovery of the hydrazine hydrate derivative was 102%~112% , and a RSD (n=12) was less than 3%. The solution used in the system was stable at 25 ℃ for 24 h with a RSD of less than 6%. The above method was applied in the detection of three Sitagliptin Phosphate samples, and hydrazine hydrate derivative was not detected. The established method is suitable for the determination of genotoxic impurity hydrazine hydrate in Sitagliptin Phosphate with high sensitivity and good specificity. |
| Key words：Sitagliptin Phosphate; GC-MS; genotoxic impurity; hydrazine hydrate; derivatization |
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基金項目：連云港高新區科技計劃項目（ZD201917）。
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作者簡(jiǎn)介：李善金（1997—），男，江蘇南京人，碩士，研究方向：藥物分析與質(zhì)量研究（E-mail：1325816338@qq.com）。
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聯(lián) 系 人：程青芳，教授，研究方向：制藥工程方面的教學(xué)與研究（E-mail：489417058@qq.com）。
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收稿日期：2021-11-17
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