UPLC-MS/MS法测定口服银杏叶片的大鼠血浆中七种活性成分及药代动力学研究(英文)

研究目的:建立一个快速灵敏且具有专属性的体内分析方法用于银杏叶片的药代动力学研究。创新要点:运用超高压液相色谱-二级质谱连用法(UPLC-MS/MS)进行大鼠血浆中七种活性成分的测定,方法简单快速,适合于银杏叶制剂的药代动力研究。研究方法:采用液液萃取进行血浆样品处理,该方法简单且快速。采用超高压液相色谱(UPLC)进行七种活性成分分离,达到了多种成分快速分离的目的。采用二级质谱(MS/MS)进行检测,优化质谱条件,减小了内源性干扰并提高检测灵敏度。经过专属性、线性、回收率、基质效应、精密度、准确度和稳定性考察,验证了该方法的适用性。经验证,该方法适用于银杏叶片的药代动力学研究。重要结论:液液萃取处理血浆样品简单可靠,回收率稳定,无基质效应(表4)。UPLC-MS/MS能够快速、灵敏、专属性地分析大鼠血浆七种活性成分的血药浓度(表3和图3)。该方法适用于银杏叶片的七种活性成分的药代动力学研究(图4和5)。     

HPLC法测定大鼠静脉注射色胺酮的血药浓度及其药代动力学研究

目的:建立HPLC法测定静脉注射色胺酮后大鼠血浆中色胺酮的浓度,研究其在体内的药代动力学过程。方法:色谱条件:色谱柱Agilent 5 HC-C18 (250 mm×4.6 mm,5μm),流动相乙腈-水(53∶47,v∶v),流速1mL/min,紫外检测器检测波长251nm,柱温30℃。以4(3H)-喹唑酮为内标物。内标标准曲线法测定生物样品中色胺酮含量,研究其体内药代动力学。结果:色胺酮在0.06～2μg/mL线性关系良好(r=0.999 7);平均回收率大于85%,批内和批间的RSD均小于15%。大鼠静脉注射75 mg/kg的色胺酮后,其体内主要药动学参数t1/2α为0.133h,t1/2β为2.193h,AUC(0-t)为4.288mg/(L·h),MRT为1.934h。结论:试验结果表明本法操作简单,灵敏度高,重现性良好,结果准确可靠,可以用于色胺酮在大鼠体内的药代动力学参数研究。     

HPLC-MS/MS法测定食品接触材料中四溴双酚A的含量

通过HPLC-MS/MS外标定量法测定食品接触材料中四溴双酚A含量,食品接触材料经剪碎后,采用甲醇超声萃取,滤膜过滤后得到待测样品。研究仪器条件、预处理工艺条件、加标回收率等因素对四溴双酚A测定的影响。结果表明,该分析方法平均加标回收率和相对标准偏差分别为84.2%～106.3%和1.8%～4.4%(n=6),适合检测现有材料中四溴双酚A的含量。优化了色谱柱、流动相和质谱参数、萃取溶剂等条件,降低了方法的检出限,提高了检测方法的灵敏度。该方法能够快速、准确检测塑料食品接触材料中四溴双酚A含量,可为食品质量监测提供技术保障。     

Determination of risperidone in human plasma by HPLC-MS/MS and its application to a pharmacokinetic study in Chinese volunteers

This study presents a rapid, specific and sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay for determination of risperidone (RIS) in human serum using paroxetine as an internal standard (IS). An Alltima-C 18separation. The analysis was performed by selected reaction monitoring (SRM) method, and the peak area of the m/z 411.3→ 191.1 transition for RIS was measured versus that of the m/z 330.1→192.1 transition for IS to generate the standard curves. The assay linearity of RIS was confirmed over the range 0.25～50.00 ng/ml and the limit of quantitation was 0.05 ng/ml. The linear range corresponds well with the serum concentrations of the analytes obtained in clinical pharmacokinetic studies. Intraday and interday relative standard deviations were 1.85%～9.09% and 1.56%～4.38%, respectively. The recovery of RIS from serum was in the range of 70.20%～84.50%. The method was successfully applied to investigate the bioequivalence between two kinds of tablets (test versus reference products) in 18 healthy male Chinese volunteers. The result suggests that two formulations are bioequivalent.