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HPLC-波长切换法同时测定消栓肠溶胶囊中7个成分的含量



        陈 玮(皖北煤电集团总医院药剂科,安徽 宿州 234000)
              *

        中图分类号 R927.2         文献标志码 A           文章编号 1001-0408(2019)17-2343-05
        DOI  10.6039/j.issn.1001-0408.2019.17.08


        摘  要   目的:建立同时测定消栓肠溶胶囊中7个活性成分绿原酸、苦杏仁苷、芍药苷、阿魏酸、洋川芎内酯Ⅰ、毛蕊异黄酮苷和藁
        本内酯的含量。方法:采用高效液相色谱法,色谱柱为Agilent Eclipse Plus C18,流动相为乙腈-0.1%磷酸溶液,梯度洗脱,检测波长
        为326 nm(绿原酸)、210 nm(苦杏仁苷)、230 nm(芍药苷)、321 nm(阿魏酸)、334(洋川芎内酯Ⅰ)、274 nm(毛蕊异黄酮苷)、260 nm
       (藁本内酯),流速为1.0 mL/min,柱温为35 ℃,进样量为10 μL。结果:绿原酸、苦杏仁苷、芍药苷、阿魏酸、洋川芎内酯Ⅰ、毛蕊异
        黄酮苷和藁本内酯检测质量浓度的线性范围分别为 1.16~34.81、1.85~55.48、13.22~396.50、13.50~405.09、1.75~52.51、2.74~
        82.18、7.67~230.07 μg/mL(r为0.999 1~0.999 7);定量限分别为0.056、0.103、0.085、0.013、0.136、0.184、0.276 μg;精密度、稳定性
       (24 h)、重复性试验的 RSD<2.0%(n=6);平均回收率分别为 99.3%、98.6%、98.8%、99.7%、97.1%、97.6%和 99.2%(RSD<
        2.0%,n=6)。结论:建立的含量测定方法操作简便、结果准确,可用于消栓肠溶胶囊中7个成分的同时测定。
        关键词 消栓肠溶胶囊;绿原酸;苦杏仁苷;芍药苷;阿魏酸;洋川芎内酯Ⅰ;毛蕊异黄酮苷;藁本内酯;含量测定;高效液相色谱法

        Simultaneous Determination of 7 Constituents in Xiaoshuan Enteric-coated Capsules by HPLC-wavelength
        Switching Method

        CHEN Wei(Dept. of Pharmacy,Wanbei Coal-electricity Corporation General Hospital,Anhui Suzhou 234000,
        China)

        ABSTRACT    OBJECTIVE: To establish a method for simultaneous determination of 7 active constituents in Xiaoshuan
        enteric-coated capsules,such as chlorogenic acid,amygdalin,paeoniflorin,ferulic acid,senkyunolide Ⅰ,calycosin glycoside and
        ligustilide. METHODS:HPLC method was adopted. The determination was performed on Agilent Eclipse Plus C18 column with
        mobile phase consisted of acetonitrile-0.1% phosphoric acid(gradient elution). The detection wavelengths were set at 326 nm for
        chlorogenic acid,210 nm for amygdalin,230 nm for paeoniflorin,321 nm for ferulic acid,334 nm for senkyunolideⅠ,274 nm
        for calycosin glycoside and 260 nm for ligustilide. The flow rate was set at 1.0 mL/min,and the column temperature was 35 ℃.
        The sample size was 10 μL. RESULTS:The linear range was 1.16-34.81 μg/mL for chlorogenic acid,1.85-55.48 μg/mL for
        amygdalin,13.22-396.50 μg/mL for paeoniflorin,13.50-405.09 μg/mL for ferulic acid,1.75-52.51 μg/mL for senkyunolideⅠ,
        2.74-82.18 μ g/mL for calycosin glycoside,7.67-230.07 μ g/mL for ligustilide (r=0.999 1-0.999 7),respectively. The limit of
        quantity were 0.056,0.103,0.085,0.013,0.136,0.184 and 0.276 μg. RSDs of precision,stability(24 h)and reproducibility tests
        were lower than 2.0%(n=6). Average recoveries were 99.3%,98.6%,98.8%,99.7%,97.1%,97.6% and 99.2%(RSD<2.0%,
        n=6). CONCLUSIONS:Established method is accurate and simple. It can be used for simultaneous determination of 7 constituents
        in Xiaoshuan enteric-coated capsules.
        KEYWORDS     Xiaoshuan enteric-coated capsules;Chlorogenic acid;Amygdalin;Paeoniflorin;Ferulic acid;Senkyunolide Ⅰ ;
        Calycosin glycoside;Ligustilide;Content determination;HPLC


            消栓肠溶胶囊具有补气、活血和通络之功效,是由                         洋川芎内酯Ⅰ可加速部分药物透过血脑屏障,具有抗血
        黄芪、当归、赤芍、川芎、地龙、桃仁和红花等7味药材制                         小板聚集和抗凝血的作用 ,绿原酸具有较广泛的抗菌、
                                                                                  [7]
                [1]
        成的制剂 。研究表明,该药对脑梗死和缺血性中风气                           抗病毒、抑制血小板聚集等作用 。方中黄芪能利水消
                                                                                       [8]
        虚血瘀症效果明显        [2-3] 。川芎-当归药对是治疗缺血性中              肿、生津养血,主要含有黄酮类和三萜皂苷类化合物,其
        风的高频用药,在治疗缺血性中风中协同发挥活血通络                           中毛蕊异黄酮苷是黄酮类典型代表化合物                    [9-10] ;方中赤
        之功用,宋代《太平惠民和剂局方》中记载的芎归汤即由                          芍可以散瘀止痛和清热凉血,内含大量单萜类化合物,
        二者组成    [4-5] ,其内在活性成分主要为绿原酸、洋川芎内                  其中以芍药苷占比较大           [11-12] ;方中桃仁主要活性成分为
                               [6]
        酯Ⅰ、阿魏酸和藁本内酯等 。据文献报道,藁本内酯和                          苦杏仁苷,具有抗动脉粥样硬化及免疫调节等作用 。在
                                                                                                     [13]
                                                                                [1]
           *主管药师。研究方向:医院药学。E-mail:51492050@qq.com          消栓肠溶胶囊现行标准 中,仅以黄芪甲苷作为定量考
        中国药房    2019年第30卷第17期                                             China Pharmacy 2019 Vol. 30 No. 17  ·2343  ·
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