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目的:针对个别企业使用不符合中国药典要求的原料非法投料生产消旋山莨菪碱片的情况,建立HPLC法测定消旋山莨菪碱片的特定杂质阿托酸6β-羟基-3α-托品酯,以监督和促使生产企业规范投料。方法:采用SHISEIDO CAPCELL C_(18)(250 mm×4.6 mm,5μm)色谱柱,以0.01 mol·L~(-1)磷酸二氢钾溶液(含0.15%三乙胺,以磷酸调节p H 6.5)-甲醇(70∶30)为流动相,流速1.0 m L·min~(-1),检测波长220 nm,柱温35℃,进样量20μL。结果:杂质阿托酸6β-羟基-3α-托品酯质量浓度在4.52~45.2μg·m L~(-1)范围内线性关系良好,回归方程为Y=19.88X+0.945 8,r=1.000,高、中、低浓度的回收率(n=3)分别为99.0%、99.2%、99.0%,RSD分别为0.1%、0.8%、0.6%。230批样品均检出该杂质,其中部分批次该杂质的含量较高。结论:该方法经方法学验证,可用于监督和促使生产企业在消旋山莨菪碱片生产过程中规范投料。
OBJECTIVE: To establish a HPLC method for the determination of racemic anisodamine hydrochloride, a specific impurity of atropine 6β-hydroxy-3α-tropicol ester, for the production of racemic anisodamine tablets by some enterprises using illegally feedstocks that do not meet the requirements of the Chinese Pharmacopoeia , In order to supervise and encourage the production enterprises to regulate the materials. METHODS: SHISEIDO CAPCELL C_ (18) (250 mm × 4.6 mm, 5 μm) column was used with 0.01 mol·L -1 potassium dihydrogen phosphate solution containing 0.15% triethylamine and phosphoric acid to adjust p H 6.5 ) -methanol (70:30) as the mobile phase at a flow rate of 1.0 m L · min -1 with a detection wavelength of 220 nm and a column temperature of 35 ° C. The injection volume was 20 μL. Results: The linearity of impurity atrophain 6β-hydroxy-3α-tropicone was good in the range of 4.52-45.2μg · m L -1 with the regression equation of Y = 19.88X + 0.945 8, r = 1.000 (N = 3) were 99.0%, 99.2% and 99.0%, respectively. The RSDs were 0.1%, 0.8% and 0.6% respectively. 230 batches of samples were detected in the impurity, some batches of the impurity content is higher. Conclusion: This method is validated by methodology and can be used to supervise and encourage manufacturers to regulate feedstocks in the production of racemic anisopamine tablets.