论文部分内容阅读
目的:建立测定杯(6)芳烃磺酸钠的含量及有关物质的高效液相色谱方法。方法:采用SHISEIDO CAPCELL ADME S5(250 mm×4.6 mm,5.0μm)色谱柱;流动相A为乙腈,流动相B为10 mmol·L-1磷酸氢二铵+10 mmol·L-1磷酸二氢铵,p H 7.0;梯度洗脱(0~30 min,2%A→21.5%A;30~35 min,21.5%A→2%A);流速:1.0 m L·min-1,检测波长:208 nm;柱温:35℃;进样体积:20μL。结果:在上述色谱条件下,各杂质及各降解产物均可与杯(6)芳烃磺酸钠主峰良好分离,主要有关物质杯(4)芳烃磺酸钠与主峰分离良好;HPLC测定的线性范围为0.1~2μg(r=0.999 0),方法的仪器精密度、日内精密度、日间精密度及重复性的RSD均小于2%;3批杯(6)芳烃磺酸钠原料药中杯(6)芳烃磺酸钠含量范围为98.14%~98.65%之间,总有关物质含量不高于1.0%。结论:经方法学验证,本法可用于测定杯(6)芳烃磺酸钠的含量及有关物质。
Objective: To establish a HPLC method for the determination of sodium (6) arene sulfonate content and related substances. METHODS: A SHISEIDO CAPCELL ADME S5 (250 mm × 4.6 mm, 5.0 μm) column was used. The mobile phase A was acetonitrile and the mobile phase B was 10 mmol·L -1 diammonium hydrogen phosphate + 10 mmol·L -1 dihydrogen phosphate Ammonium, p H 7.0; gradient elution (0-30 min, 2% A → 21.5% A; 30-35 min, 21.5% A → 2% A); flow rate: 1.0 m L · min- 208 nm; column temperature: 35 ° C; injection volume: 20 μL. Results: Under the above chromatographic conditions, all the impurities and degradation products were well separated from the main peak of arene (6) arene sulphonate, and the main related substances were cup (4) were separated from the main peak. The linear range (R = 0.999 0). The RSD of instrument precision, intra-day precision, intra-day precision and repeatability were both less than 2%. Three batches of cup (6) 6) Aromatics sulfonate content in the range of 98.14% to 98.65%, the total content of less than 1.0% of related substances. Conclusion: This method can be used to determine the content of cup (6) arene sulfonate and its related substances by methodological verification.