摘要
为建立同时测定杞菊叶黄素酯颗粒中绿原酸、木犀草苷、异绿原酸A含量的测定方法.本研究采用高效液相色谱法,用Amethyst C18-H(4.6 mm×250 mm,5μm)作为色谱柱,选择乙腈-0.1%磷酸水溶液为流动相进行梯度洗脱,检测波长348 nm,柱温25 ℃,进样量2 μL.结果显示,绿原酸、木犀草苷、异绿原酸A分别在0.01~0.07 mg/mL、0.01~0.05 mg/mL、0.03~0.16 mg/mL范围内与峰面积呈良好的线性关系,相关系数分别为0.999 4、0.999 5、0.999 2;平均回收率分别为101.33%、95.31%、109.60%,相对标准偏差为1.59%、1.29%、1.42%;精密度试验结果相对标准偏差(RSD)分别为1.01%、0.73%和0.45%;稳定性试验结果相对标准偏差为1.49%、1.26%、0.72%.该方法测得3批产品中绿原酸、木犀草苷、异绿原酸A的含量均值为(98.94±0.56)mg/100 g、(90.45±0.82)mg/100 g、(145.63±2.21)mg/100g(n=9).本研究方法简便、准确、可靠,可作为杞菊叶黄素酯颗粒的含量测定方法.
Abstract
To establish a method for the simultaneous determination of chlorogenic acid,luteolin glycoside and isochlorogenic acid A in Qiju lutein ester granules.HPLC was performed with Amethyst C18-H(4.6 mm × 250 mm,5 μm)as the chromatographic column,acetonit-rile-0.1%phosphoric acid aqueous solution was selected as the mobile phase for gradient elution,the detection wavelength was 348nm,and the column temperature was 25 ℃,injection volume was 2 μL.Chlorogenic acid,luteolin and isochlorogenic acid A showed good linear relationship with peak area in the range of 0.01~0.07 mg/mL,0.01~0.05 mg/mL and 0.03~0.16 mg/mL,respectively,and the correlation coefficients were 0.999 4,0.999 5 and 0.999 2,respectively;the average recoveries were 101.33%,95.31%and 109.60%,and the relative standard deviations were 1.59%,1.29%and 1.42%,respectively;the relative standard deviations(RSDs)of precision test results were 1.01%,0.73%and 0.45%,respectively;the relative standard deviations(RSDs)of stability test results were 1.49%,1.26%and 0.72%.The average con-tents of chlorogenic acid,luteolin and isochlorogenic acid A in three batches of products were(98.94±0.56)mg/100 g,(90.45±0.82)mg/100 g and(145.63±2.21)mg/100 g(n=9).The method in this study is simple,accurate and reliable,and can be used for the content determination of Qiju lutein ester granules.
基金项目
吉林省科学技术厅项目(20210204172YY)