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

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

作　　者：杨鹏[1] 付恩桃 高方圆[2] 范国荣[1,2] 

机构地区：[1]福建中医药大学药学院药物制剂教研室,福建福州350108 [2]第二军医大学药学院药物分析学教研室/上海市药物(中药)代谢产物研究重点实验室,上海200433

出　　处：《广东药学院学报》2014年第3期309-313,共5页Academic Journal of Guangdong College of Pharmacy

摘　　要：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。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.

关 键 词：HPLC-PDA-ESI-ITMSn 氯唑沙宗 SD大鼠 尿液 代谢产物 

分 类 号：R969[医药卫生—药理学]