连翘含量测定方法优化及青(老)翘质量控制标准建立探讨

Optimization of method for determination of Forsythia Fructus and discussion on the establishment of quality control standard for green(old) Forsythia Fructus

为了优化连翘含量测定方法,该文首先通过《中国药典》含量测定方法对各种连翘供试品的制备方法进行了评价,优选出了供试品的制备方法,即30倍70%甲醇超声提取0.5 h。该方法可满足同时提取连翘酯苷A和连翘苷的要求,并能达到最佳效果。其次,通过方法学考察建立了同时测定连翘酯苷A和连翘苷的HPLC方法,色谱条件乙腈（A）-0.4%冰醋酸溶液（B）梯度洗脱,0~33 min,15%A,33~43 min,15%~25%A,43~60 min,25%A;检测波长为277,330 nm。最后,利用该文方法和《中国药典》方法对10份青翘和5份老翘的连翘酯苷A和连翘苷进行了含量测定。结果表明：该文所建立的HPLC测定方法有效、快速、简便,符合含量测定要求。同时发现连翘酯苷A和连翘苷的含量在青翘和老翘中具有显著性差异,因此,建议两者指标成分的限量值应分别制订。该研究结果为连翘药材含量测定方法的建立和青（老）翘质量控制标准分别建立提供了依据。

In order to obtain the optimum method for content determination of Forsythia Fructus（FF）,a variety methods for the sample preparation of FF were evaluated by the content determination methods of Chinese Pharmacopoeia. And an optimum method was screened and as follows： 30 times with 70% ethanol solution in ultrasonic extractor for half an hour. The method can achieve the best effect of simultaneously extracting forsythoside A and forsythin. Then,a HPLC method for simultaneous determination of forsythoside A and forsythin was established by methodology. The HPLC chromatographic conditions： the mobile phase consisted of acetonitrile（A）-0. 4% acetic acid solution（B） with gradient elution [0-33 min,15% A,33-43 min,15%-25% A,43-60 min,25% A] was at the flow rate of 1 m L·min^-1,the column temperature was 25 ℃,and the detection wavelength was 330 and 277 nm. Moreover,the contents of forsythoside A and forsythin for 10 Green Forsythia Fructus（GF） and 5 Old Forsythia Fructus（OF） were determined by this method and Chinese Pharmacopoeia. The result not only displayed that the established method is effective,rapid,and simple,but also showed that the contents of forsythoside A and forsythin for GF and OF were significantly different. Which implied that the forsythoside A and forsythin limit standard for GF and OF should be controled by different values. This studies provide an important basis for the establishment of the content determination of FF and the quality control standard for GF and OF.