[關(guān)鍵詞]
[摘要]
目的 建立毛細(xì)管電泳法測(cè)定(S)-2-(6-羥基-2,3-二氫苯并呋喃-3-基)乙酸甲酯中R異構(gòu)體的方法。方法 采用毛細(xì)管電泳法。以磺酸-β-環(huán)糊精(S-β-CD)為選擇劑;25 mmol/L硼酸鹽緩沖液(pH 8.9,含S-β-CD 1.8%)為運(yùn)行緩沖液;運(yùn)行電壓為25 kV;柱溫為15℃;檢測(cè)波長(zhǎng):214 nm;3.4 kPa壓力進(jìn)樣10 s。結(jié)果 (S)-2-(6-羥基-2,3-二氫苯并呋喃-3-基)乙酸甲酯與R異構(gòu)體的分離度為2.9。R異構(gòu)體在2~30 μg/mL與峰面積線(xiàn)性關(guān)系良好(r=0.999 5),平均回收率為96.6%,RSD值為4.9%(n=6)。結(jié)論 建立的毛細(xì)管電泳法操作簡(jiǎn)便,結(jié)果準(zhǔn)確可靠,可用于(S)-2-(6-羥基-2,3-二氫苯并呋喃-3-基)乙酸甲酯中R異構(gòu)體的控制。
[Key word]
[Abstract]
Objective To establish a capillary electrophoresis method for the determination of R-optical isomer in (S)-methyl-2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate. Methods Capillary electrophoresis method was adopted. Sulfate-β-cyclodextrin (S-β-CD) was used as selector. The background buffer was 25 mmol/L borate buffer solution (pH 8.9, containing 1.8% S-β-CD). The separation was performed at 15 ℃ with the voltage of 25 kV and the wavelength was 214 nm. Pressure was 3.4 kPa and injected for 10 s. Results (S)-methyl-2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate and its R-enantiomer were basely resolved with resolution of 2.9. The calibration curve of R-enantiomer was linear in the concentration range of 2 - 30 μg/mL (r = 0.999 5). The average recovery was 96.6% with RSD 4.9% (n = 6). Conclusion The method is convenient, rapid, accurate, and can be used for the determination of (R)-methyl-2-(6-hydroxy-2,3-dihydrobenzofuran-3-yl)acetate in (S)-methyl-2-(6-hydroxy-2,3-dihydrobenzofuran- 3-yl) acetate.
[中圖分類(lèi)號(hào)]
[基金項(xiàng)目]
山東省自然科學(xué)基金杰出青年基金資助項(xiàng)目(JQ201319);山東大學(xué)自主創(chuàng)新基金資助項(xiàng)目(2016JC018)