摘要
目的：建立金荞麦片中6个多酚类成分（原儿茶酸、儿茶素、表儿茶素及原花青素B1、B2、C1）含量的同时测定方法。方法：采用反相高效液相色谱法,使用Shim-pack VP-ODS C18（250 mm×4.6 mm,5μm）色谱柱,流动相为乙腈与磷酸水溶液（用磷酸调p H=3.0）,梯度洗脱,流速1.0 m L·min-1,检测波长220 nm。样品采用10%乙腈回流提取。结果：6个多酚类成分分离良好,阴性无干扰,其平均加样回收率（n=6）为95.4%~104.8%（RSD为1.3%~4.6%）;重复性RSD（n=5）为1.3%~3.5%;原儿茶酸、儿茶素、表儿茶素及原花青素B1、B2、C1的线性范围分别为0.013~0.065、0.024~0.121、0.058~0.288、0.033~0.164、0.080~0.402、0.035~0.177μg,r2分别为1.000 0、0.999 9、0.999 9、0.999 8、0.999 8、0.999 0;供试品溶液中各成分在24 h内稳定。3批样品中原儿茶酸、儿茶素、表儿茶素及原花青素B1、B2、C16个成分的总含量分别为2 451.85、1 965.32、2 570.28μg·片-1。结论：新建立的方法经方法验证,可有效控制金荞麦片的质量,也可作为提高标准中新的含量测定方法。
Objective： To develop a method for simultaneous determination of six polyphenols（ protocatechuic acid,catechin,epicatechin,and procyanidins B1,B2,C1） in Jinqiaomai tablets. Methods： An HPLC method was adopted for the analysis,which was performed on a Shim- pack VP- ODS C18（ 250 mm × 4. 6 mm,5 μm） column with the mobile phase of acetonitrile and phosphoric acid solution（ p H = 3. 0） in a gradient elution,the flow rate was 1. 0 m L·min- 1,and the detection wavelength was 220 nm. The samples were pre- processed with 1 h reflux in 10% acetonitrile solution. Results： The six polyphenols were separated perfectly by chromatography without disturbing peaks from negative samples. Their average recoveries were 95. 4%- 104. 8%（ RSD 1. 3%- 4. 6%,n = 6）,the repeatabilities were expressed by RSD with values of 1. 3%- 3. 5%（ n = 6）,and linearity ranges of protocatechuic acid,catechin,epicatechin and procyanidins B1,B2,C1 were respectively 0. 013- 0. 065 μg（ r2= 1. 000 0）,0. 024-0. 121 μg（ r2= 0. 999 9）,0. 058- 0. 288 μg（ r2= 0. 999 9）,0. 033- 0. 164 μg（ r2= 0. 999 8）,0. 080- 0. 402 μg（ r2= 0. 999 8）,0. 035- 0. 177 μg（ r2= 0. 999 0）. The six polyphenols in the sample solution were stable within 24 h. The total contents of protocatechuic acid,catechin,epicatechin,and procyanidins B1,B2,C1 in 3 batches of Jinqiaomai tablets were respectively 2 451. 85 μg per tablet,1 965. 32 μg per tablet,2 570. 28 μg per tablet. Conclusion： The methodology validation proved the developed method can effectively control the quality of Jinqiaomai tablets,and can be used as a new assay method in the quality standard as well.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第4期644-648,共5页
Chinese Journal of Pharmaceutical Analysis
关键词
金荞麦片
原儿茶酸
儿茶素
表儿茶素
原花青素
高效液相色谱法
方法验证
Jinqiaomai tablets
protocatechuic acid
catechin
epicatechin
procyanidin
RP-HPLC method
methodology validation
