高效液相色谱法测定GL-V9的含量和有关物质  

Determination of related substances and content of GL-V9 by HPLC

作　　者：张丽莹 杨越莛 沈经纬 柳文媛[1] ZHANG Li-ying;YANG Yue-ting;SHEN Jing-wei;LIU Wen-yuan(Department of China Pharmaceutical University,Nanjing 211198)

机构地区：[1]中国药科大学药物分析系,南京211198

出　　处：《中南药学》2020年第4期656-661,共6页Central South Pharmacy

摘　　要：目的建立GL-V9含量和有关物质测定的HPLC法,并进行全面的方法学验证。方法采用RPHPLC法测定GL-V9的含量,并对其有关物质进行检测。色谱柱为ODS-3(4.6 mm×150 mm,5μm),甲醇-乙腈-10 mmol·L^-1磷酸铵(用磷酸调节pH值至3.2)为流动相,梯度洗脱,流速1.0 mL·min^-1,柱温30℃,检测波长274 nm。结果在含量测定色谱条件下,GL-V9浓度在1.98~19.82μg·mL^-1与峰面积呈良好线性关系(r=1.000);在有关物质测定色谱条件下,有关物质汉黄芩素、GLV9-Z8、GLV9-Z10分别在质量浓度0.0505~0.4039μg·mL^-1(r=0.9997)、0.1936~1.9362μg·mL^-1(r=0.9999)、0.1902~1.9021μg·mL^-1(r=0.9998)与峰面积呈良好的线性关系;汉黄芩素、GLV9-Z8、GLV9-Z10总含量分别为0.02%、0.03%、0.24%。结论本方法专属性好、准确可靠、灵敏度高、重现性好,可用于GL-V9有关物质的检测分析及质量控制。Objective To establish an HPLC method to determine related substances and content of GL-V9.Methods RP-HPLC was adopted to determine GL-V9,and related substances with an ODS-3 C18 column(150 mm×4.6 mm,5μm)with a gradient elution system of acetonitrile-methanol-10 mmol·L^-1 ammonium phosphate(adjusting the pH to 3.2 with phosphoric acid).The column temperature was maintained at 30℃,the flow rate was 1.0 mL·min^-1,and the detection wavelength was 274 nm.Results For the content determination,a linearity between the area and concentration of GL-V9 was achieved at 1.98-19.82μg·mL^-1(r=1.000).For the determination of impurities,the standard curves of wogonin,GLV9-Z8 and GLV9-Z10 were linear at 0.0505-0.4039μg·mL^-1(r=0.9997),0.1936-1.9362μg·mL^-1(r=0.9999),and 0.1902-1.9021μg·mL^-1(r=0.9998),respectively.The contents of wogonin,GLV9-Z8,and GLV9-Z10 were 0.02%,0.03%,and 0.24%,respectively.Conclusion The determination method for related substances and content is sensitive,reproducible,accurate and reliable.It could be applied in the analysis of related substances and quality control of GL-V9 in the raw materials.

关 键 词：GL-V9 有关物质 含量测定 反相高效液相色谱法 

分 类 号：R927[医药卫生—药学]