双波长HPLC法同时测定两面针药材中5种成分的含量
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篇名: 双波长HPLC法同时测定两面针药材中5种成分的含量
TITLE:
摘要: 目的:建立同时测定两面针药材中5种成分含量的方法。方法:采用高效液相色谱法。色谱柱为Luna C18,流动相为乙腈-水(含0.2%磷酸、0.25% 三乙胺)(梯度洗脱),流速为1.0 mL/min,检测波长为273、284 nm,柱温为30 ℃,进样量为20 μL。结果:别隐品碱、盐酸血根碱、氯化两面针碱、白屈菜红碱、芝麻素检测质量浓度线性范围分别为0.8~200、0.2~50、0.44~110、0.208~52、0.944~236 μg/mL(r均为0.999 9);精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为101.47%~103.92%(RSD=0.92%,n=9)、102.52%~104.68%(RSD=0.63%,n=9)、97.55%~101.22%(RSD=1.09%,n=9)、103.35%~104.93%(RSD=0.71%,n=9)、99.31%~103.86%(RSD=1.34%,n=9)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于两面针药材中5种成分含量的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for the simultaneous determination of 5 components in Zanthoxylum nitidum. METHODS: HPLC was performed on the column of Luna C18 with mobile phase of acetonitrile-water (containing 0.2% phosphoric acid, 0.25% triethylamine) (gradient elution) at a flow rate of 1.0 mL/min, detection wavelength was 273, 284 nm, column temperature was 30 ℃, and the injection volume was 20 μL. RESULTS: The linear range was 0.8-200 μg/mL for allocryptopine (r=0.999 9), 0.2-50 μg/mL for sargentine hydrochloride (r=0.999 9), 0.44-110 μg/mL for nitidine chloride (r=0.999 9), 0.208-52 μg/mL for toddaline (r=0.999 9) and 0.944-236 μg/mL for sesamin (r=0.999 9); RSDs of precision, stability and reproducibility tests were lower than 2.0%; recoveries were 101.47%-103.92% (RSD=0.92%,n=9), 102.52%-104.68% (RSD=0.63%,n=9), 97.55%-101.22% (RSD=1.09%,n=9), 103.35%-104.93% (RSD=0.71%,n=9), 99.31%-103.86% (RSD=1.34%,n=9). CONCLUSIONS: The method is simple with good precision, stability and reproducibility, and can be used for the simultaneous determination of 5 components in Z. nitidum.
期刊: 2017年第28卷第3期
作者: 孙科,陈冉,陆世惠
AUTHORS: SUN Ke,CHEN Ran,LU Shihui
关键字: 高效液相色谱法;两面针;别隐品碱;盐酸血根碱;氯化两面针碱;白屈菜红碱;芝麻素;含量
KEYWORDS: HPLC; Zanthoxylum nitidum; Allocryptopine; Sargentine hydrochloride; Nitidine chloride; Toddaline; Sesamin; Content
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