摘要
目的:建立 HPLC 法同时测定肿节风中异嗪皮啶-7-O-β-D-葡萄糖苷、异嗪皮啶和山柰酚-3-O-β-D-葡萄糖酸苷的含量。方法:色谱柱:Waters XBridge C_(18)柱(250 mm×4.6 mm,5μm);流动相:0.1%醋酸甲醇溶液(A)-0.1%醋酸水溶液(B),梯度洗脱(0~17 min,A:25%,B:75%;17~65 min,A:25%→55%,B:75%→45%);流速为0.5 mL·min^(-1);检测波长为344 nm;柱温26℃。结果:异嗪皮啶-7-O-β-D-葡萄糖苷、异嗪皮啶和山柰酚-3-O-β-D-葡萄糖酸苷的线性范围分别为0.2~4.0μg(r=0.9999),0.2~4.0μg(r=0.9999),0.5~10μg(r=0.9999);平均回收率(n=5)分别为100.6%(RSD=1.7%),99.8%(RSD=1.1%),99.6%(RSD=0.4%)。结论:所建立的 HPLC 方法操作简便,准确可靠,分离度好,为全面评价肿节风药材的质量提供了实验依据。
Objective:To establish an HPLC method for simultaneous determination of isofraxidin -7 - O -β - D - glucopyranoside, isofraxidin, and kaempferol - 3 - O -β- D - glucuronid in Sarcandra glabra ( Thunb. ) Nakai. Method:HPLC with Waters XBridge C18 column(250 mm ×4.6 mm,5 μm). The mobile phase was 0. 1% acetic acid in methanol (A) and 0. 1% acetic acid water solution (B) with gradient elution mode at the flow rate of 0. 5 mL · min ^-1. The gradient condition was 0 - 17 min, A : 25% , B : 75% ; 17 - 65 min, A : 25% →55% , B : 75%→ 45%. The detection wavelength was 344 nm. Column temperature :26 ℃. Results:The linear ranges of isofraxidin - 7 - O - β - D - glucopyranoside, isofraxidin and kaempferol - 3 - O - β - D - glucuronid were 0. 2 - 4.0 μg ( r = 0. 9999) ,0.2 - 4. 0 μg ( r = 0. 9999 ), 0.5 - 10 μg ( r = 0. 9999 ), respectively. The average recoveries were 100.6% ( RSD = 1.7 % ), 99. 8 % ( RSD = 1.1% ), 99.6 % ( RSD = 0. 4 % ), respectively. Conclusion: This method is simple, sensitive and reliable, and it can provide an experimental basis for quality evaluation of Sarcandra glabra (Thunb.) Nakai.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第9期1481-1484,共4页
Chinese Journal of Pharmaceutical Analysis
基金
浙江省科技厅重点科技攻关项目(2006C23008)