摘要
建立HPLC 法同时测定党参中烟酸及党参炔苷含量的方法.采用Syncronis AQ 色谱柱(250 mm×4.6mm,5 μm),以乙腈(A)–0.2% 磷酸水溶液(B) 作流动相进行梯度洗脱,流量为1 mL/min,紫外检测波长为285 nm,柱温为30 ℃,烟酸和党参炔苷可在24 min 内实现与其它成分良好分离.烟酸的质量浓度在9.6~57.6 μg/mL 范围内与色谱峰面积线性关系良好(r=0.999 2),检出限为0.94 μg/mL,测定结果的相对标准偏差为1.5%(n=6),平均加标回收率为99.5% ;党参炔苷的质量浓度在9.92~59.52 μg/mL 范围内与色谱峰面积线性关系良好(r=0.999 6),检出限为0.12 μg/mL,测定结果的相对标准偏差为1.9%(n=6),平均加标回收率为101.1%.该方法操作简便、快速、准确,具有良好的重复性,可作为党参中烟酸、党参炔苷测定的有效方法.
A HPLC method was established for the determination of nicotinic acid and lobetyolin in Codonopsis pilosula. A Syncronis AQ column(250 mm×4.6 mm,5 μm) was used with acetonitrile(A)–0.2% phosphoric acid solution(B) as the mobile phase at the flow rate of 1 mL/min,the detection wavelength was set at 285 nm and the column temperature was kept at 30℃. The results showed that nicotinic acid and lobetyolin could be separated within 24 min. The mass concentration of nicotinic acid had good linearity with chromatographic peak area in the range of 9.6–57.6 μg/mL(r=0.999 2), and the detection limit was 0.94 μg/mL,the relative standard deviation of determination results was 1.5%(n=6),the average recovery was 99.5%. The mass concentration of lobetyolin had good linearity with chromatographic peak area in the range of 9.92–59.52 μg/mL(r=0.999 6), and the detection limit was 0.12 μg/mL,the relative standard deviation of determination results was 1.9%(n=6),the average recovery was 101.1%. The method is convenient,rapid,accurate,which can be applied to the determination of nicotinic acid and lobetyolin in Codonopsis pilosula.
出处
《化学分析计量》
CAS
2016年第3期12-15,共4页
Chemical Analysis And Meterage
基金
科技部"重大新药创制"科技重大专项(2014ZX09509001–001)
山东省高校中医药抗病毒协同创新中心(XTCX2014C01–02)
关键词
党参
烟酸
党参炔苷
HPLC
Codonopsis pilosula
nicotinic acid
lobetyolin
HPLC