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目的建立同时测定苦黄注射液中生物碱和大黄蒽醌类成分的定量分析方法。方法采用Venusil MP C_(18)(2)(4.6 mm×250 mm,5μm)色谱柱为分析柱,甲醇(A)-0.4%二乙胺(B),梯度洗脱(A为5%→5%→40%→60%→80%→5%,相应时间周期为0→5→20→30→55→60 min),流速为1.0 m L·min~(-1),紫外检测波长为254 nm,柱温位30℃。结果在选定色谱条件下,芦荟大黄素、大黄酸、苦参碱、大黄素、大黄酚、氧化苦参碱、大黄素甲醚、槐定碱、槐果碱分别在0.012 3~0.369μg、0.023~0.69μg、0.138~4.14μg、0.056~1.68μg、0.065~1.95μg、0.145~4.35μg、0.012 5~0.375μg、0.146~4.38μg和0.101~3.03μg内线性关系良好(r=0.999 3,0.999 6,0.999 6,0.999 6,0.999 4,0.999 3,0.999 5,0.999 4,0.999 4),加样回收率分别为98.38%,100.79%,98.03%,99.81%,98.62%,99.28%,98.90%,101.75%,100.75%,RSD分别为1.60%,2.65%,2.12%,2.78%,2.08%,2.45%,2.08%,2.35%,1.72%。结论该方法操作简便易行,重复性好,结果准确可靠,可为苦黄注射液的质量控制提供定量评价方法。
Objective To establish a quantitative method for simultaneous determination of alkaloids and anthraquinones in Kuhuang injection. Methods A Venusil MP C_ (18) (2) (4.6 mm × 250 mm, 5 μm) column was used as the analytical column. The column was eluted with methanol (A) -0.4% diethylamine % → 40% → 60% → 80% → 5%, the corresponding time period is 0 → 5 → 20 → 30 → 55 → 60 min), the flow rate is 1.0 m L · min -1 and the UV detection wavelength is 254 nm, column temperature 30 ℃. Results Under the selected chromatographic conditions, the contents of aloe-emodin, rhein, matrine, emodin, chrysophanol, oxymatrine, physcion, sophoridine and sophocarpine were respectively 0.012 3 ~ 0.369 μg, (R = 0.999 3, 0.013-0.46 μg, 0.138-4.14 μg, 0.056-1.68 μg, 0.065-1.95 μg, 0.145-4.35 μg, 0.012 5-0.375 μg, 0.146-4.48 μg and 0.101-3.0 μg, respectively) 0.999 6,0.999 6,0.999 6,0.999 4,0.999 3,0.999 5,0.999 4,0.999 4) The recoveries of samples were 98.38%, 100.79%, 98.03%, 99.81%, 98.62%, 99.28%, 98.90 %, 101.75%, 100.75%, RSD 1.60%, 2.65%, 2.12%, 2.78%, 2.08%, 2.45%, 2.08%, 2.35%, 1.72% respectively. Conclusion The method is simple and easy to operate with good repeatability and accurate and reliable results. It can provide a quantitative evaluation method for the quality control of Kuhuang injection.