复方大黄灌肠液的质量考察

Study on the quality standard of compound Rhubarb fluid enema

目的:制定复方大黄灌肠液(大黄、乌梅)的质量标准。方法:采用薄层色谱法鉴别处方中大黄、乌梅二味中药材,采用高效液相法对大黄5种蒽醌成分进行含量分析,采用色谱柱:WondaSil Superb C18(4.6 mm×250 mm,5μm),流动相:甲醇-0.1%磷酸水溶液(84∶16),检测波长:254 nm,流速:1.0mL·min-1。柱温:30℃。采用高效液相法对乌梅中柠檬酸进行含量分析,采用色谱柱:WondaSil Superb C18(4.6 mm×250 mm,5μm),流动相:甲醇-0.1%磷酸水溶液(5∶95),检测波长:214 nm,流速:0.5 mL·min-1。,柱温:25℃。结果:薄层色谱斑点清晰,分离度好,阴性无干扰;大黄蒽醌成分(芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚)的线性范围分别为0.20～6.34 mg·L-1(r=0.999 9),0.40～12.67 mg·L-1(r=0.999 9),0.41～13.12 mg·L-1(r=0.999 9),0.41～12.99 mg·L-1(r=0.999 9),0.45～14.40 mg·L-1(r=0.999 9),平均回收率(n=6)分别为96.02%,96.49%,96.73%,102.42%,97.47%,RSD分别为0.40%,1.98%,0.81%,2.25%,2.11%。柠檬酸的线性范围分别为22.10～265.20 mg·L-1(r=0.999 9),加样回收率为100.57%,RSD为2.43%。结论:定性定量分析方法快速、准确、专属性强,本法可控制复方大黄灌肠液的质量。

OBJECTIVE To establish the compound Rhubarb enema （Radix et Rhizoma Rhei, Fructus Mume） quality stand- ards. METHODS TLC was used to distinguish the prescription of Rhubarb, Fructus Mume two herbs. The contents of 5 kinds of anthraquinone components in Rhubarb were analyzed by HPLC. WondaSil Superb Cls （4. 6 minx 250 ram, 5 μm） was used as chromatographic column; mobile phase： methanol-0. 1% of phosphoric acid water solution （84 ： 16）, the detection wave- length： 254 nm, flow rate： 1.0 mL · min-1 The column temperature： 30 ~C. An HPLC method was used for content analysis of citric acid in Fruetus mume, by using chromatographic column： WondaSil Superb C18 （4. 6 ram· 250 mm,5 μm）, mobile phase： methanol-0. 1% of phosphoric acid water solution （5：95）, the detection wavelength： 214 nm, flow rate： 0. 5 mL· rain -1, column temperature： 25 ℃. RESULTS The TLC spots were clear, the separation degree was good, no negative inter- ference; the linear range of 5 kinds of anthraquinone （aloe emodin, rheim emodin, ehrysophanol, physcion） was 0. 20-6. 34 mg.L I（r=0.999 9）, 0. 40-12.67 mg·L-1（r=0.999 9）, 0.41-13. 12 mg·L-1（r=0.999 9）, 0.41-12.99 mg·L-1（r= 0. 999 9）, 0. 45- 14. 40 mg ·L -1 （r = 0. 999 9） respectively, the average recovery rate （n = 6） was 96.02%, 96. 49%, 96.73%, 102.42% ,97. 47% respectively, RSD were 0.40%, 1.98%, 0. 81%, 2. 25%, 2.11%. The linear range of citrate was 22. 1（1-265.20 mg·L-1 （r= 0. 999 9）, the average recovery was 100. 57%, RSD was 2. 43%. CONCLUSION Qualitative and quantitative analysis method is rapid, accurate, reproducible, this method can be used as the quality standard of Compound Rhubarb enema.