LC-MS/MS测定人尿中匹诺塞林浓度及尿排泄研究  

Determination of Pinocembrin in Human Urine by LC-MS/MS and Research on Urinary Excretion

作　　者：严蓓[1] 曹国颖[1] 闫记灵[2] 胡欣[1] 彭悦颖[2] 边子睿[2] 李可欣[1] 

机构地区：[1]北京医院药学部临床药理室、药物临床风险与个体化应用评价北京市重点实验室,北京100730 [2]石药集团中奇制药技术石家庄有限公司,石家庄050051

出　　处：《中国药学杂志》2014年第17期1540-1544,共5页Chinese Pharmaceutical Journal

基　　金：国家科技部“重大新药创制”科技重大专项(2012ZX09303008-002);国家自然科学基金资助项目(81202601)

摘　　要：目的 建立高效液相色谱-串联质谱（LC-MS/MS）测定人尿中匹诺塞林浓度,考察其在中国健康受试者尿液中的排泄特征。方法 尿样用乙醚液-液萃取,采用LunaTMC8色谱柱（2.00 mm×150 mm,3μm）分离,以乙腈-0.3 mmol·L-1醋酸铵水溶液（65∶35,V/V）为流动相进行等度洗脱,流速为0.25 mL·min-1,通过电喷雾离子源（ESI）,多重反应监测（MRM）负离子模式进行检测。8名受试者静脉滴注匹诺塞林40 mg,测定匹诺塞林的尿药排泄参数。结果 匹诺塞林在3~200 ng·mL-1内线性关系良好,定量下限为3 ng·mL-1,批内、批间变异（RSD）小于6.34%,稳定性较好。受试者给药后,匹诺塞林在给药结束后4 h尿的累积排泄百分率达到平台,48 h累计排泄百分率为（0.11±0.05）%。结论 该方法快速、灵敏、准确、专属性强、重现性高,适用于人尿中匹诺塞林的测定及其尿药排泄特征研究。OBJECTIVE To develop a liquid chromatography-tandem mass spectrometry （LC-MS/MS） method for determination of pinocembrin in human urine, and to investigate its urinary excretory after intravenous drip administration of pinocembrin in healthy volunteers. METHODS The urine samples were extracted with ether. The separation was performed on a Luna C8 column （2. 00 mm × 150 mm, 3 μm） using the mobile phase composed of acetonitrile-0. 3 mmol · L-1 ammonium acetate solution （65： 35, V/V） at a flow rate of 0. 25 mL · min- 1 in isocratic mode. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring （MRM） via electrospray ionization （ESI） source in negative mode. Urinary excretion parameters were cal- culated after a single intravenous drip administration of pinocembrin at 40 mg to humans. RESULTS The assay was linear from 3 ng · mL-1 to 200 ng · mL-1, with the lower limit of quantification at 3 ng · mL-1. The within-run and between-run precision （RSD） were below 6. 34%. Pinocembrin had good stability. At 4 h after the completion of administration, the urinary cumulative excretion percentage reached a plateau and the cumulative excretion percentage in urine within 48 h were （0. 11 ± 0. 05 ） %. CONCLUSION This method is rapid, sensitive, accurate, specific and reliable, and suitable for the determination of pinocembrin in human urine and for the investigation to the urinary excretion.

关 键 词：高效液相色谱-串联质谱法 匹诺塞林 尿药排泄 

分 类 号：R285.5[医药卫生—中药学]