一测多评法同时测定咽炎片中5种指标性成分的含量 点击下载
论文标题: 一测多评法同时测定咽炎片中5种指标性成分的含量
英文标题:
中文摘要: 目的:建立一测多评法同时测定咽炎片中芍药苷、芦丁、木蝴蝶苷B、黄芩苷、肉桂酸等5种指标性成分的含量。方法:采用高效液相色谱法。色谱柱为Hypersil GOLD-C18(250 mm×4.6 mm,5 μm),流动相为甲醇-0.35%磷酸水溶液(梯度洗脱),检测波长为280 nm(芦丁、木蝴蝶苷B、黄芩苷、肉桂酸)、230 nm(芍药苷),柱温为30 ℃,流速为1 mL/min,进样量为10 μL。以芍药苷为内参物,建立芦丁、木蝴蝶苷B、黄芩苷、肉桂酸的相对校正因子;考察不同色谱系统、色谱柱、流动相比例、流速、柱温对相对校正因子的影响,并按相对保留时间对待测成分进行色谱峰定位。按外标法测定内参物芍药苷含量,按一测多评法测定其余4种成分含量,并与外标法测定结果进行比较。结果:各待测成分的分离度均大于1.5;芍药苷、芦丁、木蝴蝶苷B、黄芩苷、肉桂酸的质量浓度分别在3.97~119.22、1.96~58.68、2.39~71.64、1.92~57.51、0.54~16.24 μg/mL范围内线性关系良好(r≥0.999 7);精密度、重复性、稳定性试验的RSD均小于2%;平均加样回收率为97.20%~98.07%(RSD<3%,n=6)。以芍药苷为内参物,芦丁、木蝴蝶苷B、黄芩苷、肉桂酸的平均相对校正因子分别为0.554 6、1.815 6、2.489 3、5.423 2;在不同色谱条件下其相对校正因子和相对保留时间的RSD均小于5%。采用一测多评法与外标法分别测得10批咽炎片待检样品中4种成分(除内参物外)含量的相对误差绝对值均小于1%,两种方法测定结果一致。结论:本方法准确、快捷、高效、价廉,可用于同时测定咽炎片中5种指标性成分的含量。
英文摘要: OBJECTIVE: To establish QAMS method for content determination of paeoniflorin, rutin, oroxin B, baicalin and cinnamates in Yanyan tablets. METHODS: HPLC method was adopted. The determination was performed on Hypersil GOLD-C18 column (250 mm×4.6 mm,5 μm) with mobile phase consisted of methanol-0.35% phosphoric acid solution (gradient elution) at flow rate of 1 mL/min. The detection wavelengths were set at 280 nm (rutin, oroxin B, baicalin, cinnamates) and 230 nm (paeoniflorin). The column temperature was 30 ℃, and sample size was 10 μL. Using paeoniflorin as internal reference, relative correction factors (RCF) of rutin, oroxin B, baicalin and cinnamates were established. Effects of different chromatogram system, chromatogram column, mobile phase proportion, flow rate and column temperature on relative correction factors were investigated; the chromatographic peaks of the components were located according to the relative retention time. The content of paeoniflorin as internal reference was determined by external standard method, and the other four components were determined by QAMS, and then compared with the results of external standard method. RESULTS: The separation degree of each component to be measured was greater than 1.5. The linear range was 3.97-119.22 μg/mL for paeoniflorin,1.96-58.68 μg/mL for rutin,2.39-71.64 μg/mL for oroxin B, 1.92-57.51 μg/mL for baicalin, 0.54-16.24 μg/mL for cinnamates(r≥0.999 7), respectively. RSDs of precision, reproducibility and stability tests were all lower than 2%. Average recoveries were 97.20%-98.07%(RSD<3%,n=6). RCFs of rutin, oroxin B, baicalin and cinnamates were 0.554 6,1.815 6,2.489 3 and 5.423 2, using paeoniflorin as internal reference. RSDs of RCF and relative retention time were all lower than 5% under different chromatogram conditions. Absolut relative error of four components (except for internal reference) in 10 batches of Yanyan tablets sampled by QAMS and external standard method were all less than 1%. The results of the two methods were identical. CONCLUSIONS: The established method is accurate, rapid, efficient and inexpensive, and it can be used for simultaneous determination of 5 indicator components in Yanyan tablet.
期刊: 2019年第30卷第16期
作者: 马昌豪,李怀伟,仝桂平,马海春,冯思腾
英文作者: MA Changhao, LI Huaiwei, TONG Guiping, MA Haichun, FENG Siteng
关键字: 咽炎片;一测多评法;芍药苷;芦丁;木蝴蝶苷B;黄芩苷;肉桂酸;高效液相色谱法;含量测定
KEYWORDS: Yanyan tablet; QAMS; Paeoniflorin; Rutin; Oroxin B; Baicalin; Cinnamates; HPLC; Content determination
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