| 第 50 卷第 3 期 |  | Vol. 50 No. 3 | | 2020 年 6 月 | Jun 2020 |
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所屬欄目：分析與測試
頂空氣相色譜法測定異丁司特原料藥中有機溶劑的殘留量 |
| 付丙月1，崔新強1，吳偉山2，王金虎1*
（1. 山東省藥學(xué)科學(xué)院 山東省化學(xué)藥物重點(diǎn)實(shí)驗室，山東 濟南 250101；2. 山東省中醫藥大學(xué) 附屬醫院骨科，山東 濟南 250011） |
| 摘 要：以Agilent DB-624毛細管柱為色譜柱，程序升溫，氫火焰離子化檢測器，采用頂空氣相色譜法。建立同時(shí)測定異丁司特原料藥中乙醇、二氯甲烷、正己烷、乙酸乙酯、四氫呋喃、甲苯六種有機溶劑殘留量的方法。在此色譜條件下，乙醇、二氯甲烷、正己烷、乙酸乙酯、四氫呋喃、甲苯這六種待測有機殘留溶劑的分離度均大于1.5，空白溶劑無(wú)干擾，線(xiàn)性、準確度、精密度良好。該方法操作簡(jiǎn)單，重復性好，適用于異丁司特原料藥中六種有機溶劑殘留的同時(shí)測定。 |
| 關(guān)鍵詞：異丁司特；氣相色譜法；頂空進(jìn)樣；有機溶劑殘留 |
| 中圖分類(lèi)號：O657.7 文獻標識碼：A 文章編號：1009-9212（2020）03-0069-04 |
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| Determination of Organic Solvent Residual in Ibudilast by Headspace Gas Chromatography |
| FU Bing-yue1, CUI Xin-qiang1, WU Wei-shan2, WANG Jin-hu1*
(1. Shandong Provincial Key Laboratory of Chemical Drugs Shandong Academy of Pharmaceutical Sciences, Jinan 250101, China; 2. Affiliated Hospital of Shandong University of Traditional Chinese Medicine Department of Orthopedics, Jinan 250011, China) |
| Abstract：In this headspace gas chromatography method, the Agilent DB-624 capillary column was used as the chromatographic column, the temperature was programmed and the hydrogen flame ionization detector was used. To establish a method for the simultaneous determination of the residuals of six kinds of organic solvents including ethanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, and toluene in Ibudilast. Under this chromatographic condition, the resolution of the organic solvents including ethanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, and toluene were all greater than 1.5, while the blank solvent had no interference, and the linearity, accuracy, and precision were good. This method was proved to be simple, repeatable, and suitable for the simultaneous determination of 6 organic solvent residues in Ibudilast. |
| Key words：ibudilast; gas chromatography; headspace sampling; residual organic solvents |
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基金項目：山東省重大科技創(chuàng )新工程項目（2019JZZY010520）。
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作者簡(jiǎn)介：付丙月（1985-），女，山東濟南人，碩士，主要從事新藥研發(fā)和藥物分析（E-mail：fubingyue-2004@163.com）。
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聯(lián) 系 人：王金虎，副主任藥師，主要從事藥物分析（E-mail：wjh1573@126.com）。
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收稿日期：2020-05-21
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