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15-甲基前列腺素 F-2α临床试用于早期引产已多年,为有效控制其质量,需对其 R、S差向异构体进行定量分析。由于本品在近紫外区无明显吸收峰,一般高压液相层析难以得到满意的结果。作者将本品溶于对溴基溴化苯乙酮的乙腈溶液中并用二异丙基乙胺作催化剂,在室温反应制成前列腺素的对溴苯酰甲基衍生物,在波长约256 nm 处有强吸收,不仅用紫外分光光度检测器可灵敏检测,且有利于改进色谱分离效果。方法采用正相高压液相层析法,在无定形微粒硅胶柱(silica A)上用醋酸乙酯:氯仿(1:1,为缩短分析时间,亦可3:1)混合液洗脱,R、S 差向异构体可完全分离,可满足定量测定要求,尚可分离若干杂质。本品衍生物制备在室温即可顺利进行,勿需特殊处理。经试验,室温反应1小时,98%以上本品已定量转化为衍生物,此衍生物在反应液内可稳定6小时以上。经用普通柱层析分离制备对溴基苯酰甲基15-S-甲基前列腺素 F-2α纯品结晶,mp85～86 C,高压液相层析呈
The clinical trial of 15-methyl prostaglandin F-2α has been used for many years in the early induction of labor. To effectively control its quality, it is necessary to quantitatively analyze the R and S epimers. Because this product has no obvious absorption peak in the near-ultraviolet region, high-pressure liquid chromatography is generally difficult to obtain satisfactory results. The authors dissolved the product in acetonitrile solution of p-bromo bromide acetophenone and used diisopropylethylamine as a catalyst to react at room temperature to prepare p-bromobenzoylmethyl derivatives of prostaglandins at a wavelength of about 256 nm. With strong absorption, it is not only sensitive to UV spectrophotometric detectors, but also helps improve chromatographic separation. Methods Normal phase high-pressure liquid chromatography was used to elute the mixture of ethyl acetate:chloroform (1:1, shortening the analysis time, also 3:1) on the amorphous silica gel column (silica A). R The S and the epimers can be completely separated to meet the requirements of quantitative determination, and several impurities can be separated. The preparation of this product can be smoothly performed at room temperature without special treatment. After testing, the reaction at room temperature for 1 hour, more than 98% of the product has been quantitatively converted to a derivative, this derivative can be stable in the reaction solution for more than 6 hours. The pure p-bromobenzoylmethyl 15-S-methylprostaglandin F-2α crystals were isolated by ordinary column chromatography and the mp was 85-86 C.