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目的建立大鼠尿、粪便中狼毒色原酮含量测定的方法,并考察其排泄特征。方法采用高效液相色谱-质谱联用法测定给药后大鼠尿、粪中狼毒色原酮的含量,分别计算狼毒色原酮在尿、粪便中的累积排泄量及排泄率。色谱条件:XbridgeTM C18(2.1 mm×50 mm,3.5μm,Waters柱,流动相为0.1%甲酸甲醇-0.1%甲酸水溶液梯度洗脱,流速0.4 mL·min-1,电喷雾型质谱检测器,采用MRM方式同时进行测定;用于定量分析的离子反应分别为:狼毒色原酮(m/z 543.3→198.9),瑞舒伐他汀(m/z 481.9→258.3)。结果在8~6 400 ng·mL-1狼毒色原酮在尿液和粪便复溶液中线性良好(r2≥0.999 5,n=5),最低检测限为4 ng·mL-1。低、中、高浓度的质控样品日内、日间精密度和准确度均符合要求。灌胃给予狼毒色原酮后48 h的尿、粪便中累积排泄率分别为(1.84±0.290)%、(41.5±6.917)%。结论所建立的分析方法准确、灵敏、快速,符合生物样品分析要求,适用于粪便、尿液中狼毒色原酮的分析。排泄实验结果表明,粪便是狼毒色原酮的最主要的排泄方式。
Objective To establish a method for the determination of eradication of rubetrone in rat urine and faeces and investigate its excretion characteristics. Methods The content of luteinone in rat urine and feces was determined by high performance liquid chromatography-mass spectrometry. The cumulative excretion and excretion rate of luteinone in urine and feces were calculated. Chromatographic conditions: XbridgeTM C18 (2.1 mm × 50 mm, 3.5 μm, Waters column, mobile phase gradient 0.1% formic acid-0.1% formic acid in water, flow rate 0.4 mL · min -1, electrospray mass spectrometry detector MRM method were used for the simultaneous determination.The ion reactions for quantitative analysis were astrotrin (m / z 543.3 → 198.9) and rosuvastatin (m / z 481.9 → 258.3) · ML-1 eugenolone showed good linearity (r2 ≥ 0.999 5, n = 5) in urine and stool reconstituted solution with the lowest detection limit of 4 ng · mL-1. The control of low, medium and high concentrations The intra-day and inter-day precision and accuracy of the samples met the requirements, and the cumulative excretion rates in urine and faeces were (1.84 ± 0.290)% and (41.5 ± 6.917)%, respectively, 48 hours after gavage. The established analytical method is accurate, sensitive and rapid, and meets the requirements of biological sample analysis.It is suitable for the analysis of eradication of lanuginasterone in excrement and urine.The excretion experiment shows that excrement is the most important excretion way .