Valtrate is the main drug quality control for the qualitative and quantitative analysis of Valerian medicines in the Chinese Pharmacopoeia 2010. However, valtrate is unstable under some conditions. We, for the first time, systemically evaluated the stability of two bath reference standards （RS） by high performance liquid chromatography coupled with a triple quadrupole mass spectrometer （HPLC-MS/MS）. The forced degradations of valtrate were performed to evaluate its optimal storage, transportation and experiment conditions according to ICH guideline. The developed HPLC method was validated to determine the degradation products. Valtrate RS was sensitive to alkaline and thermal conditions, but it was relatively stable under acidic, oxidation and photolysis conditions. A total of nine degradation components were identified under alkaline hydrolysis （N1-N4） and thermal degradation （B1-B5）. The information obtained in this work would be valuable to minimize the decomposition of valtrate during the processes of preparation, storage, distribution and utilization. It was highly suggested to store valtrate with a single dose packing in brown closed ampoule at -20℃. Under the above-mentioned storage condition, valtrate could be stable for up to 3 years.
目的通过高效液相色谱-二极管阵列检测-串联质谱（HPLC-DAD-MS/MS）法结合谱库筛查龙血竭、红花、跌打丸、二十五味珊瑚丸、跌打活血散中21种合成染料（金胺O、金橙Ⅱ、胭脂红等）。方法 7批阳性样品甲醇或乙醇提取液的分析采用Phenomenon Luna C18色谱柱（250 mm×4.6 mm,5μm）;以乙腈-0.05 mol/L醋酸铵为流动相,梯度洗脱;体积流量1 m L/min;柱温40℃;检测波长400~700 nm。MS分析采用ESI电离源;干燥气温度350℃,体积流量10 L/min;雾化气压力241.3 k Pa;源电压4 k V。结果所有样品均检测出合成染料,谱库匹配度均大于99.8。结论该方法准确快速,可用于中药中合成染料筛查。
