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目的建立解毒剂量甘草和中毒剂量马钱子药材提取液混合物的高效液相色谱-紫外-串联质谱(HPLC-UV-MS)分析方法,并运用于甘草和马钱子大鼠口服入血成分分析。方法采用Sino Chrome ODS-BP(4.6 mm×250 mm,5μm)色谱柱,水(含0.1%甲酸)(A)-乙腈(B)(V/V)为流动相,梯度洗脱:0.01 min 8%B,2 min 8%B,30 min 25%B,32 min 30%B,50 min45%B,53 min 85%B,60 min 85%B,61 min 8%B,77 min停止,流速0.3 mL·min~(-1)。UV检测波长254 nm,柱温40℃。质谱扫描采用正负离子模式同时检测的全扫描模式,正负离子模式锥孔电压分别30、25 V,毛细管电压分别为2.5、3.5 V。待测血浆用乙腈沉淀蛋白处理后测定。结果建立了同时测定甘草和马钱子药材提取物及入血成分的HPLC-UV-MS方法,比较了甘草和马钱子体内外物质变化。结论采用简便,可重复的HPLC-UV-MS方法对甘草和马钱子提取物体内外成分进行确证和分析,为甘草对马钱子解毒机制的物质基础研究提供实验依据。
OBJECTIVE To establish a HPLC-UV-MS method for determination of detoxification dose of Glycyrrhiza uralensis and poisoned Strychnos nux vomica extract mixture, . Methods The mobile phase consisted of Sino Chrome ODS-BP (4.6 mm × 250 mm, 5 μm) column, water (containing 0.1% formic acid) and acetonitrile (B) % B 2 min 8% B 30 min 25% B 32 min 30% B 50 min 45% B 53 min 85% B 60 min 85% B 61 min 8% B 77 min Stop flow 0.3 mL · min ~ (-1). UV detection wavelength 254 nm, column temperature 40 ℃. The mass spectrometry scan was performed in both positive and negative mode with full scan mode. The positive and negative cone mode voltage was 30 and 25 V, respectively, and the capillary voltage was 2.5 and 3.5 V, respectively. The plasma to be tested is treated with acetonitrile precipitated protein. Results HPLC-UV-MS method was established for the simultaneous determination of extracts and blood components of licorice root and Strychnos nux-vomica. The changes of substance in vitro and in vivo were compared. Conclusion The simple and reproducible HPLC-UV-MS method was used to confirm and analyze the in vitro and in vivo components of licorice and strychnos extract, which provided the experimental basis for the material basis of licorice root detoxification mechanism.