| 第 53 卷第 3 期 |  | Vol. 53 No. 3 | | 2023 年 6 月 | Jun 2023 |
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所屬欄目：分析與測試
手性HPLC法分析雙乙�？屏弱τ钞悩嬻w |
| 趙春影1，2，王淑紅2，崔佰吉1，楊威龍1，孟繁偉1，蔡建輝1，修志明1*
（1. 吉林醫藥學(xué)院，吉林 吉林 132013；2. 長(cháng)春百純和成醫藥科技有限公司，吉林 長(cháng)春 130012） |
| 摘 要：建立了前列腺素中間體雙乙�？屏弱τ钞悩嬻w的手性高效液相色譜測定方法。采用硅膠表面涂覆有纖維素-三（3，5-二甲基苯基氨基甲酸酯）的手性色譜柱（OD-H，4.6 mm×250 mm，5 μm），以正己烷-異丙醇（V∶V=80∶20）為流動(dòng)相，流速1.0 mL/min，柱溫40 ℃，檢測波長(cháng)205 nm，外標法測定對映異構體超量值。結果雙乙�？屏弱τ钞悩嬻w分離度為3.5，（+）-雙乙�？屏弱ピ�0.199~3.980 mg/mL（R2=0.999 4）、（-）-雙乙�？屏弱ピ�0.198~3.960 mg/mL（R2=0.999 4）濃度范圍線(xiàn)性關(guān)系良好。（+）-雙乙�？屏弱サ�、中、高濃度平均加樣回收率（RSD）分別為99.38%（0.43%）、99.30%（0.88%）、100.10%（0.51%），（-）-雙乙�？屏弱サ�、中、高濃度平均加樣回收率（RSD）為99.76%（0.86%）、100.07%（0.26%）、99.27%（0.20%）。3批樣品平均對映異構體超量值為4.75%、70.10%、-75.33%。方法簡(jiǎn)便、快速，能準確測定雙乙�？屏弱τ钞悩嬻w超量值，為前列腺素藥物手性中間體提供新的分離和檢測方法。 |
| 關(guān)鍵詞：HPLC；手性；雙乙�？屏弱�；對映異構體超量 |
| 中圖分類(lèi)號：R917 文獻標識碼：A 文章編號：1009-9212（2023）03-0062-06 |
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| Determination of Diacetylation Corey Lactone Enantiomers by Chiral HPLC |
| ZHAO Chun-ying1,2, WANG Shu-hong2, CUI Bai-ji1, YANG Wei-long1, MENG Fan-wei1, CAI Jian-hui1, XIU Zhi-ming1*
(1. Jilin Medical University, Jilin 132013, China; 2. Changchun BC & HC Pharmaceutical Technology Co., Ltd., Changchun 130012, China) |
| Abstract：A method for determination of the prostaglandin intermediates diacetylation corey lactone enantiomers by chiral HPLC were established. The optimal chromatographic conditions were as follows: chiral column (OD-H, 4.6 mm×250 mm, 5 μm) coated with Cellulose-tri(3,5-dimethylphenylcarbamate), mobile phase: n-hexane-isopropyl alcohol (V∶V=80∶20), flow rate 1.0 mL/min, column temperature 40 ℃, detection wavelength 205 nm, the enantiomeric excess value was calculated by external standard method. The results showed that the resolution between the corey lactone diol enantiomers was 3.5, and (+)-diacetylation corey lactone had a good linear relationship (R2=0.999 4) in the concentration range of 0.199~3.980 mg/mL as well as (-)-diacetylation corey lactone in the concentration range of 0.198~3.960 mg/mL (R2=0.999 4). The average recoveries (RSD) of (+)-diacetylation corey lactone at low, medium and high concentrations were 99.38%(0.43%), 99.30%(0.88%), 100.10%(0.51%). The average recoveries (RSD) of (-)-diacetylation corey lactone at low, medium and high concentrations were 99.76%(0.86%), 100.07%(0.26%), 99.27%(0.20%). The average enantiomeric excess values of three samples were 4.75%, 70.10%, -75.33%. The established method is simple, rapid and accurate, and can accurately determine the enantiomeric excess value of diacetylation corey lactone enantiomers. It provides a new method for the separation and detection of chiral intermediates of prostaglandin drugs. |
| Key words：HPLC; chiral; diacetylation corey lactone; enantiomeric excess |
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基金項目：吉林省科技廳項目（20200708090YY）。
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作者簡(jiǎn)介：趙春影（1978—），女，吉林松原人，工程師，研究方向：前列腺素類(lèi)藥物分析（E-mail：3464245416@qq.com）。
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聯(lián) 系 人：修志明，教授，碩士生導師，研究方向：前列腺素藥物篩選與設計（E-mail：Xiuzm10@mails.jlu.edu.cn）。
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收稿日期：2023-05-05
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