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目的:紫外分光光度法(UV)测定胃肠舒片中大黄总蒽醌的含量;高效液相色谱法(HPLC)测定制剂中大黄素、大黄酚、芦荟大黄素、大黄酸和大黄素甲醚的含量。方法:UV法利用大黄蒽醌类化合物与醋酸镁反应显色的原理,510 nm处测定其吸收度。HPLC法中色谱柱:Hypersil BDS C18(250 mm×4.6 mm,5μm),流动相:甲醇-0.1%醋酸水溶液(75∶25),流速:1.0 mL/min,检测波长:440 nm,柱温:室温。结果:紫外分光光度法在3.6～20.0μg/mL的范围内线性关系良好(r=0.9908,n=6);HPLC法中芦荟大黄素、大黄酸、大黄素、大黄酚和和大黄素甲醚进样量分别在14.7～937.5(r1=0.9987)、36.6～2 344.0(r2=0.9989)、12.2～781.3(r3=0.9992)、11.6～1 500.0(r4=0.9930)和600.0～6 250.0(r5=0.9995)ng/mL范围内与峰面积呈良好线性关系(n=6)。结论:该方法简便、精确、分离效果好、专属性强,可作为胃肠舒片的质量控制方法。
OBJECTIVE: To determine the content of total anthraquinone in rhubarb and rhubarb by UV spectrophotometry. The contents of emodin, chrysophanol, aloe-emodin, rhein and rhein in the preparations were determined by high performance liquid chromatography (HPLC) Content. Methods: UV method using anthraquinones and rhubarb reaction with the principle of magnesium acetate, 510 nm at the determination of its absorption. HPLC column: Hypersil BDS C18 (250 mm × 4.6 mm, 5 μm), mobile phase: methanol-0.1% aqueous acetic acid (75:25), flow rate 1.0 mL / min, detection wavelength 440 nm, Room temperature. Results: UV spectrophotometry showed a good linearity (r = 0.9908, n = 6) in the range of 3.6-20.0μg / mL. The results of HPLC showed that aloe-emodin, rhein, emodin, chrysophanol and emodin The injection volumes ranged from 14.7 to 937.5 (r1 = 0.9987), 36.62 344.0 (r2 = 0.9989), 12.2-781.3 (r3 = 0.9992), 11.6-1,500.0 (r4 = 0.9930) and 600.0-6 250.0 (r5 = 0.9995) ng / mL showed a good linear relationship with the peak area (n = 6). Conclusion: The method is simple, accurate, good separation effect, specificity, and can be used as a quality control method of Shuchangxu Tablet.