摘要
目的建立以高效液相色谱法测定河豚毒素原料药含量及其有关物质的方法。方法色谱柱为PhecdaDiol柱(4.6mm×250mm,5μm),流动相为乙腈-0.3%甲酸[/10mmol甲酸铵溶液(83:17)(v/v),流速为1.0mL·min-1,检测波长为196nm,柱温为30℃。结果主峰能与相邻杂质峰较好分离,TTX检测浓度的线性范围为60~40μg·mL-1(r=0.9999),检测限为10ng(S/N=3)。结论该方法简便、准确、专属性强,可用于河豚毒素的含量测定和有关物质的检查。
Objective To establish a HPLC method for the determination of tetrodotoxin (TTX) and its related substances in crude tetrodotoxin. Methods HPLC was carried out on a Phecda Diol column (4.6 mm×250 mm, 5 μm) with acetonitrile -0.3 % formic acid and 10 mmol of ammonium formate(83 : 17)(v/v ) as the mobile phase at a flow rate of 1.0 mLmin-1. The detection wavelength was 196 nm, and the column temperature was maintained at 30 ℃. Results Fair resolution between TYX and its related substances was presented in the chromatograms. The calibrated linear curve of TYX was within the range of 60~140 μg·mL-l(r=0.9999). The limit of detection(LOD) was 10 ng(S/ N=3). Conclusion The established HPLC method is accurate and reliable, and can be used for the determination of tetrodotoxin and its related substances in crude tetrodotoxin.
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2011年第4期455-458,共4页
Traditional Chinese Drug Research and Clinical Pharmacology