【摘要】 目的建立快速、简便、灵敏、准确的高效液相色谱-串联质谱(HPLC-MS)测定干蟾皮中华蟾酥毒基和酯蟾毒配基含量方法。方法采用HPLC-MS正离子多反应监测模式测定,Zorbax SB-C18液相色谱柱(50 mm×2.1 mm,1.8μm);流动相为乙腈-0.1%甲酸水溶液(41∶59),体积流量200μL/min,柱温30℃。质谱条件:氮气温度350℃,氮气体积流量12 L/min,雾化器压力为101.316 kPa(35 psi)。华蟾酥毒基碎裂电压160 V,碰撞能15 eV,母离子、子离子分别为m/z 443.2、364.8;酯蟾毒配基碎裂电压130 V,碰撞能15 eV,母离子、子离子分别为m/z 385.2、366.9。结果华蟾酥毒基和酯蟾毒配基分别在0.99～7.92μg/m L和1.04～8.32μg/m L内线性关系良好。检测限(S/N≥3)均为0.3 ng/g。华蟾酥毒基、酯蟾毒配基回收率分别为97.96%～103.7%、96.86%～102.4%。日内及日间精密度RSD均小于3%。结论所建方法灵敏、可靠,能满足干蟾皮有毒物质分析的需要。更多还原

【Abstract】 Objective To develop a rapid, simple, sensitive, and accurate high performance liquid chromatography-tandem mass spectrometry(HPLC-MS) method for determining the contents of cinobufagin and resibufogenin from Bufo Corium. Methods The contetns were determined by Zorbax SB-C18 column and tested in positive electrospray ionization with multiple reaction monitoring of HPLC-MS. The mobile phase was conswasted with the mixture of acetonitril-0.1 mol/L formic acid water solution(41∶59), flow rate200 μL/min, column temperature 30 oC. Mass spectrometry conditions: nitrogen temperature 350 oC, nitrogen flow rate 12 L/min,nebulizer pressure 101.316 kPa(35 psi). The shredded voltage of cinobufagin was 160 V, the collwasion energy was 15, the parent ion and the daughter ion were 443.2 and 364.8 respectively; The fragmentation voltage of resibufogenin was 130 V, the collwasion energy was 15, and the parent ion and the daughter ion were 385.2 and 366.9 respectively. Results There was good linearity in the range of0.99—7.92 μg/m L and 1.04—8.32 μg/mL for the cinobufagin and resibufogenin. The detection limit(S/N ≥ 3) was 0.3 ng/g. The recoveries of cinobufagin and resibufogenin ranged from 97.96% to 103.7% and 96.86% to 102.4%, respectively. The intraday and daytime precwasion were both less than 3%. Conclusion The results showed that the method was sensitive and reliable, which can meet the needs of analyse of toxic substances in B. Corium.更多还原