枳术颗粒质量标准研究

Quality standard for Zhizhu Granules

目的建立枳术颗粒(枳实、白术、荷叶)的质量控制方法。方法采用薄层色谱法鉴别本制剂中的枳实、白术、荷叶;采用高效液相色谱法测定本制剂中辛弗林、荷叶碱、柚皮苷、新橙皮苷。辛弗林色谱条件:流动相甲醇-水(含0.2%磷酸钠,0.3%十二烷基硫酸钠,用磷酸调pH值至3.5)(50∶50);检测波长275 nm。荷叶碱色谱条件:以乙腈为流动相A,以水(含2.2%三乙胺,1.1%冰醋酸)为流动相B,梯度洗脱;检测波长为270 nm。柚皮苷和新橙皮苷色谱条件:流动相乙腈-水(20:80);检测波长284 nm。结果定性鉴别方法专属性强、薄层效果佳。辛弗林的进样量在0.020 6～1.028 3μg范围内呈现良好的线性关系,相关系数r=0.999 9;荷叶碱的进样量在0.020 9～0.521μg范围内呈现良好的线性关系,相关系数r=0.999 9;柚皮苷进样量在0.377～3.770μg范围内呈现良好的线性关系,相关系数r=1.000 0;新橙皮苷进样量在0.301 6～3.016μg范围内呈现良好的线性关系,相关系数r=1.000 0。4个待测成分的平均回收率分别为99.7%、97.8%、99.9%、99.5%(RSD%均≤2.0%)。结论本方法准确可靠、重现性好,可有效控制枳术颗粒的质量。

AIM To establish the quality standard for Zhizhu Granules （Aurantii Fructus immaturus, Atrac- tylodes macrocephala Rhizoma, Nelumbinis Folium ）. METHODS In the prescription, Aurantii Fructus immatu- rus, Atractylodes macrocephala Rhizoma, Nelumbinis Folium were identified by TLC, and RP-HPLC was adopted to determine synephrine, nuciferine, naringin, neohesperidin in the granules. The chromatographic conditions of syn- ephrine included the methanol-water （ containing 0.2% Na3P04, 0.3% SDS, adjusting pH to 3.5 by H3PO4） （50 ： 50） as the mobile phase at the detection wavelength of 275 nm. Nuciferine was determined with acetonitrile-water （containing 2.2% triethylamine, 1.1% acetic acid） as gradient eluent at the detection wavelength of 270 nm. The contents of naringin and neohesperidin were determined once by HPLC with mobile phase consisting of acetonitrilewater （20 ： 80）. The UV wavelength was set at 284 nm. RESULTS The established identification methods were proper and reflecting a good specificity. The experiment showed good linear relationship at the ranges of 0.020 6- 1. 028 3 μg for synephrine, 0. 020 9-0. 521 μg for nuciferine, 0. 377-3. 770 μg for naringin, 0. 301 6- 3. 016 μg for neohesperidin （r = 0. 999 9, 0. 999 9, 1. 000 0, 1. 000 0）, respectively. In addition, the average recoveries were 99.7%, 97.8%, 99.9%, 99.5% （RSD≤2.0%）, respectively. CONCLUSION The established meth- ods are not only practical but capable of effectively controlling the quality of Zhizhu Granules.