摘要
目的建立测定去甲二氢愈创木酸(NDGA)含量和检查有关物质的HPLC方法。方法采用ZorbaxSB-C18色谱柱(4.6mm×250mm,5μm),检测波长为282nm。含量测定以三氟醋酸-水-乙腈(0.05:45:55,pH3.5)为流动相,有关物质检查采用梯度洗脱,以三氟醋酸-水(0.05:100)为流动相A,三氟醋酸-乙腈(0.05:100)为流动相B,洗脱梯度:0～15min,流动相B的比例为40%～70%,15～30min,流动相B的比例为70%。结果NDGA浓度为5.0～100.0μg/ml时,峰面积与其浓度呈良好的线性关系(r=0.9999),检测限为1.2ng(S/n=3),含量测定重复性试验RSD为0.54%(n=6)。有关物质检查重复性试验RSD1.8%(n=6)。结论本法简便、准确、快速、灵敏,可用于NDGA的质量控制。
Objective To establish HPLC methods to detect content and related substances of nordihydroguaiaretic acid （NDGA）. Methods A Zorbax SB-C18 column （4.6 mm × 250 mm, 5 μm） was used and the detection wavelength was set at 282 nm. The mobile phase for content assay was TFA-water-acetonitrile （0. 05：45：55, pH 3.5）. Detection of the related substances was carried out with gradient elution of 0.05% TFA water solution （A） and 0.05% TFA-acetonitrile solution （B） as follows： 0- 15 min, the ratio of B was 40% - 70% ; 15 - 35 min, the ratio of B was 70%. Results The calibration curve was linear （r = 0. 999 9） within the range of 5.0 -100.0 μg/ml for NDGA, the detection limit was 1.2 ng （S/n = 3）, the repeatability precision RSD was 0.54% （ n = 6 ） for NDGA, 1.8% （ n = 6） for related substances. Conclusion This method is simple, accurate, quick and sensitive, and can be applied to the quality control of NDGA.
出处
《第三军医大学学报》
CAS
CSCD
北大核心
2007年第12期1148-1151,共4页
Journal of Third Military Medical University
基金
国家"863"计划引导项目(2002AA001010)
重庆市科技攻关项目(CSTC-2005AA5007-1)~~
