HPLC-PDA-ESI-ITMS~n法鉴定氯唑沙宗在SD大鼠尿液中的代谢产物

目的通过高效液相色谱-光电二极管阵列检测器/离子阱质谱（HPLC-PDA-ESI-ITMSn）联用技术定性分析氯唑沙宗在SD大鼠尿液中的代谢产物。方法高效液相色谱条件：采用Benatnach C18（250 mm×4.6 mm,5μm）色谱柱,以甲醇-水（含10 mmol乙酸铵）进行梯度洗脱,流速为0.8 mL/min,检测波长为287 nm。ESI质谱条件：负离子扫描模式,喷针电压为5 000 V,毛细管电压为20 V,干燥气（N2）压力为137.896 kPa,质量扫描范围为m/z 50-500,雾化温度为300℃。结果通过HPLC-PDA-ESI-ITMSn联用技术,分离并鉴定出SD大鼠口服氯唑沙宗原料药后,尿液中的5种氯唑沙宗代谢产物,并揭示了这5种代谢产物的质谱裂解规律。结论本方法灵敏度高、专属性强,为氯唑沙宗在SD大鼠体内的代谢途径及代谢过程的研究提供了依据。

Identification of chlorzoxazone metabolites in SD rat urine using HPLC-PDA-ESI-ITMS~n

Objective To analyze qualitatively chlorzoxazone metabolites in SD rat urine using highperformance liquid chromatography with photodiode array detector and electrospray ionization ion trap tandem mass spectrometry（HPLC-PDA-ESI-ITMSn）.Methods The chromatographic separation was performed on a Benatnach C18（250 mm × 4.6 mm,5 μm） column with a mobile phase composed of methanol-water containing 10 mmol ammonium acetate,eluted at a flow rate of 0.8 mL/min,and UV detection wavelength was set at 287 nm.Negative ionization mode with a needle voltage of 5 000 V,a capillary voltage of 20 V,a gas（N2） press of 137.896 kPa and a temperature of the drying gas at 300 ℃ were selected.Relative molecular mass data acquisition was performed from m/z 50 to 500 in full MS scan mode.Results A total of five metabolites of chlorzoxazone were identified using HPLC-PDA-ESI-ITMSnin SD rat urine after an oral administration of chlorzoxazone.The method revealed the fragmentation pattern of chlorzoxazone metabolites.Conclusions A sensitive and specific HPLC-PDA-ESI-ITMSnmethod for identifying metabolites of chlorzoxazone has been established,which provides more scientific information for the metabolic pathways and metabolic process of chlorzoxazone.