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本文介绍用气液层析法同时测定缓冲片剂及一般片剂中阿司匹林与非阿司匹林水杨酸盐的含量,方法是在不同条件下用氯仿提取,再与双(三甲基硅烷)乙酰胺生成衍生物进行气液层析测定。实验条件:气相层析仪,自动积分仪,氢火焰电离检测器,固定柏为3％oV-17,担体为用硅烷化硅土,柱长1.8m,内径2mm,进样温度180°,柱温120°,检出器温度140°,氮气流量约35ml/分,每结束一个样品将柱温升高到240°3分钟,以冲洗层析柱。一、缓冲片剂中阿司匹林与非阿司匹林水杨酸盐测定:内标液:425mg 对羟苯酸丙酯溶于100ml 氯仿。标准液:(1)125mg 阿司匹林溶于50ml 氯仿(必须于2小时内使用);(2)15mg 水杨酸溶于200ml 氯仿。
This article describes the simultaneous determination of aspirin and non-aspirin salicylates in buffered and generic tablets by gas-liquid chromatography using chloroform extracted under different conditions followed by bis (trimethylsilyl) acetamide Derivatives were generated for gas-liquid chromatography. Experimental conditions: gas chromatography, automatic integrator, hydrogen flame ionization detector, fixed cypress 3% oV-17, the carrier for the use of silanized silica column length 1.8m, an inner diameter of 2mm, the injection temperature of 180 °, the column The temperature was 120 °, the detector temperature was 140 °, and the nitrogen flow rate was about 35 ml / min. The column temperature was raised to 240 ° for 3 minutes at each end of a sample to wash the column. First, the aspirin buffer tablets and non-aspirin salicylate determination: Internal standard solution: 425mg propylparaben dissolved in 100ml of chloroform. Standard solution: (1) 125mg aspirin dissolved in 50ml chloroform (must be used within 2 hours); (2) 15mg salicylic acid was dissolved in 200ml chloroform.