HPLC法同时测定消癌平片中通关藤苷A和通关藤苷I的含量
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篇名: HPLC法同时测定消癌平片中通关藤苷A和通关藤苷I的含量
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摘要: 目的:建立同时测定消癌平片中通关藤苷A和通关藤苷I含量的方法。方法:取消癌平片经三氯甲烷萃取后采用高效液相色谱(HPLC)法进样分析。色谱柱为Symmetry C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),检测波长为223 nm,流速为1.0   mL/min,柱温为25 ℃,进样量为20 μL。采用上述条件测定3批样品中通关藤苷A和通关藤苷I的含量。结果:通关藤苷A、通关藤苷I的质量浓度检测线性范围分别为26.40~264.00 μg/mL(r=0.999 4)、4.59~45.90 μg/mL(r=0.999 3),检测限分别为0.26、0.12 μg/mL,定量限分别为0.79、0.36 μg/mL;精密度、稳定性(12 h)、重复性试验峰面积的RSD均<2.0%(n=6);加样回收率分别为98.53%~99.28%(RSD为0.20%~0.51%,n=9)、97.00%~98.89%(RSD为0.19%~1.03%,n=9)。3批样品中通关藤苷A和通关藤苷I的含量分别为2.27~2.32、0.64~0.69 mg/g。结论:本试验建立的方法简便,结果准确可靠,适用于消癌平片中通关藤苷A和通关藤苷I含量的同时测定。
ABSTRACT: OBJECTIVE: To develop a method for simultaneous determination of tenacissoside A and tenacissoside I in Xiaoaiping tablets. METHODS: HPLC method was used to analyze Xiaoaiping tablets after extracted by trichlormethane. The determination was performed in Symmetry C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 223 nm, and the column temperature was 25 ℃. The sample size was 20 μL. The content of tenacissoside A and tenacissoside I in 3 batches of samples were determined by above condition. RESULTS: The linear range of tenacissoside A and tenacissoside I were 26.40-264.00 μg/mL (r=0.999 4) and 4.59-45.90 μg/mL (r=0.999 3), respectively. The limits of detection were 0.26, 0.12 μg/mL, and the limits of quantification were 0.79, 0.36 μg/mL. RSDs of precision, stability (12 h) and repeatability tests were all lower than 2.0%(n=6). The recoveries were 98.53%-99.28% (RSD=0.20%-0.51%,n=9) and 97.00%-98.89% (RSD=0.19%-1.03%,n=9). The contents of tenacissoside A and tenacissoside I in 3 batches of samples were 2.27-2.32 mg/g and 0.64-0.69 mg/g, respectively. CONCLUSIONS: The established method is accurate, simple and reliable, which is suitable for simultaneous determination of tenacissoside A and tenacissoside I in Xiaoaiping tablets.
期刊: 2018年第29卷第13期
作者: 王祁民,马银玲,安静,张磊,孙利民,白万军,温艳虹,董占军
AUTHORS: WANG Qimin,MA Yinling,AN Jing,ZHANG Lei,SUN Limin,BAI Wanjun,WEN Yanhong,DONG Zhanjun
关键字: 高效液相色谱法; 消癌平片; 通关藤苷A; 通关藤苷I;含量测定
KEYWORDS: HPLC; Xiaoaiping tablets; Tenacissoside A; Tenacissoside I; Content determination
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