一测多评法同时测定扶正固本颗粒中6种成分的含量
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篇名: 一测多评法同时测定扶正固本颗粒中6种成分的含量
TITLE: Simultaneous Determination of the Contents of 6 Components in Fuzheng Guben Granules by QAMS
摘要: 目的:建立扶正固本颗粒中2,3,5,4′-四羟基二苯乙烯基葡萄糖苷、黄芩苷、淫羊藿苷、汉黄芩苷、黄芩素、汉黄芩素等6种成分含量的测定方法。方法:采用高效液相色谱法。色谱柱为DikmaDiamonsilC18,流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),检测波长为275nm(0~8min)、320nm(8~9min)和275nm(9~33min),流速为1.0mL/min,柱温为25℃,进样量为10μL。以黄芩苷为基准物,采用多点校正法和斜率校正法分别计算另外5种成分的相对校正因子(fk/s),并采用保留时间差值法对待测成分进行色谱峰定位,比较上述两种一测多评法所得计算值与外标法实测值的差异。结果:2,3,5,4′-四羟基二苯乙烯基葡萄糖苷、黄芩苷、淫羊藿苷、汉黄芩苷、黄芩素、汉黄芩素检测进样量的线性范围分别为0.053~2.12、0.163~6.52、0.059~2.36、0.0216~0.864、0.03~1.2、0.021~0.84μg(r>0.999),精密度、稳定性(12h)、重复性试验的RSD均小于3%;平均加样回收率为98.72%~99.82%(RSD为0.89%~1.24%,n=9)。以黄芩苷为基准物,2,3,5,4′-四羟基二苯乙烯基葡萄糖苷、淫羊藿苷、汉黄芩苷、黄芩素、汉黄芩素多点校正法的fk/s分别为1.172、0.528、1.479、1.820、2.534,斜率校正法的fk/s分别为1.234、0.550、1.559、1.939、2.664;3种方法测得10批扶正固本颗粒中6种成分含量的RSD为0.29%~2.77%(n=10);两种一测多评法测得结果与外标法的Pearson相关系数均不低于0.9999(P<0.001)。结论:成功建立了可用于同时测定扶正固本颗粒中6种成分含量的一测多评法。
ABSTRACT: OBJECTIVE:To establish the method for content determination of 6 components in Fuzheng guben granules ,such as 2,3,5,4′-tetrahydroxystilbene glucoside ,baicalin,icariin,scutellarin,baicalein and wogonin. METHODS :HPLC method was adopted. The determination was performed on Dikma Diamonsil C 18 column with mobile phase consisted of acetonitrile- 0.1% phosphoric acid aqueous solution (gradient elution )at the flow rate of 1.0 mL/min. The detection wavelengths were set at 275 nm (0-8 min),320 nm(8-9 min)and 275 nm(9-33 min). The column temperature was set at 25 ℃,and sample size was 10 μL. With baicalin as reference material ,the relative corr ection factors (fk/s) of other five components were calculated by multi-point correction method and slope correction method ;the retention time difference method was used to locate the chromatographic peaks ; the calculation values obtained by above 2 QAMS were compared with measured values of external standard method. RESULTS : The linear range of 2,3,5,4′-tetrahydroxystilbene glucoside ,baicalin,icariin,scutellarin,baicalein and wogonin were 0.053-2.12, 0.163-6.52,0.059-2.36,0.021 6-0.864,0.03-1.2,0.021-0.84 μg(r>0.999),respectively. RSDs of precision ,stability(12 h)and reproducibility tests were all lower than 3%. Average recoveries were 98.72%-99.82%(RSDs were 0.89%-1.24%,n=9). Using baicalin as reference material ,fk/s of multi-point correction method for 2,3,5,4′-tetrahydroxystilbene glucoside ,icariin,scutellarin, baicalein and wogonin were 1.172,0.528,1.479,1.820 and 2.534,respectively;fk/s of slope correction method were 1.234, 0.550,1.559,1.939,2.664. RSDs of 6 components in 10 batches of Fuzheng guben granules by 3 methods were 0.29%-2.77% (n=10),respectively. Pearson correlation coefficient was not lower than 0.999 9(P<0.001)in measured values between QAMS and external standard method. CONCLUSIONS :QAMS method is established successfully for simultaneous determination of 6 components in Fuzheng guben granules.
期刊: 2021年第32卷第02期
作者: 仝立国,牛艳艳,王若瑜,吉海杰,宋美卿,冯玛莉,夏召弟,汪欣文
AUTHORS: TONG Liguo,NIU Yanyan ,WANG Ruoyu ,JI Haijie,SONG Meiqing ,FENG Mali,XIA Zhaodi ,WANG Xinwen
关键字: 一测多评法;扶正固本颗粒;2,3,5,4′-四羟基二苯乙烯基葡萄糖苷 ;黄芩苷;淫羊藿苷;汉黄芩苷;黄芩素;汉黄芩素;
KEYWORDS: QAMS;Fuzheng guben granules ;2,3,5,4′-tetrahydroxystilbene glucoside ;Baicalin;Icariin;Scutellarin;Bai-
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