高效液相色谱-电雾式检测器法同时测定川芎茶调颗粒中7个活性成分  

Simultaneous determination of seven active ingredients in Chuanxiong Chatiao Granules by HPLC-CAD

作　　者：刘群 王磊 肖云娜 LIU Qun;WANG Lei;XIAO Yun-na(Yantai Center for Food and Drug Control and Test,Shandong Yantai 264003,China)

机构地区：[1]烟台市食品药品检验检测中心,山东烟台264003

出　　处：《中国医院药学杂志》2021年第14期1417-1422,共6页Chinese Journal of Hospital Pharmacy

摘　　要：目的:建立高效液相色谱法联合电雾式检测器同时测定川芎茶调颗粒中阿魏酸、甘草酸、阿魏酸松柏酯、洋川芎内酯A、Z-藁本内酯、欧前胡素及异欧前胡素的含量。方法:采用Agilent Eclipse XDB-C_(18)(250 mm×4.6 mm,5μm)色谱柱,以10 mmol·L^(-1)甲酸铵(A)-80%乙腈(B)为流动相,梯度洗脱,流量1.0 mL·min^(-1),柱温35℃,CAD雾化器温度为35℃,采集频率10 Hz,过滤常数5.0。结果:阿魏酸、甘草酸、阿魏酸松柏酯、洋川芎内酯A、Z-藁本内酯、欧前胡素及异欧前胡素的质量浓度分别在0.55~17.50(r=0.9999),5.90~295.00(r=0.9999),2.51~125.50(r=0.9999),5.02~251.00(r=0.9999),4.99~249.50(r=0.9999),1.03~51.50(r=0.9998)及0.59~29.50μg·mL^(-1)(r=0.9998)内线性关系良好;平均加样回收率分别为97.78%,97.76%,97.54%,98.09%,97.98%,97.89%及98.05%,RSD(n=6)分别为0.96%,1.50%,0.84%,1.49%,1.50%,1.37%及1.65%;方法精密度、重复性和溶液稳定性均符合规定。10批样品中上述7个成分含量范围分别为0.45~0.60,4.93~6.20,2.01~2.73,2.63~3.43,4.72~5.70,1.13~1.84及0.38~0.52 mg/袋。结论:经方法学验证,本方法准确性好,灵敏度高,简便易行,可用于川芎茶调颗粒中多指标成分的质量控制研究。OBJECTIVE To develop an HPLC-CAD method for simultaneous determination of seven active ingredients of ferulic acid,glycyrrhizic acid,coniferly ferulate,senkyunolide A,Z-ligustilide,imperatorin and isoimperatorin in Chuanxiong Chatiao Granules.METHODS Chromatographic separation was performed on an Agilent Eclipse XDB-C18(250 mm×4.6 mm,5μm)column with 10 mmol·L^(-1) ammonium formate(A)-80%acetonitrile(B)as the mobile phase for gradient elution,flow rate of 1.0 mL·min^(-1),column temperature of 35℃,nebulization temperature of detector 35℃,acquisition frequency 10 Hz and filtration constant 5.0.RESULTS Ferulic acid,glycyrrhizic acid,coniferly ferulate,senkyunolide A,Z-ligustilide,imperatorin and isoimperatorin were linear in the ranges of 0.55-11.00μg·mL-1(r=0.9993),5.90-118.00μg·mL^(-1)(r=0.9994),2.51-50.20μg·mL^(-1)(r=0.9995),5.02-100.40μg·mL^(-1)(r=0.9994),4.99-99.80μg·mL^(-1)(r=0.9998),1.03-20.60μg·mL^(-1)(r=0.9995)and 0.59-11.80μg·mL-1(r=0.9995)respectively;The average recoveries were 97.78%,97.76%,97.54%,98.09%,97.98%,97.89%and 98.05%and RSDs 0.96%,1.50%,0.84%,1.49%,1.50%,1.37%and 1.65%respectively.Precision,reproducibility and stability of solution were in accord with the regulations.The content ranges of seven ingredients were 0.45-0.60,4.93-6.20,2.01-2.73,2.63-3.43,4.72-5.70,1.13-1.84 and 0.38-0.52 mg/bag.CONCLUSION The above method is accurate,sensitive,convenient and reproducible for quality control of multicomponents in Chuanxiong Chatiao Granules.

关 键 词：电雾式检测器 川芎茶调颗粒 阿魏酸 甘草酸 阿魏酸松柏酯 洋川芎内酯A Z-藁本内酯 欧前胡素 异欧前胡素 含量测定 

分 类 号：R284[医药卫生—中药学]