静脉滴注入血白蛋白注射液致急性肾功能衰竭1例

病例:患者,女,64岁,因"直肠癌"于2007年4月27日在我院手术治疗.术后恢复尚可,无明显转移征象,肝、肾功能正常.术后尿常规示:pH5.9,尿蛋白(-),大便黄软,镜检(-),食欲欠佳,住院31天出院.

Liquid chromatography electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) method for quantitative estimation of moxifloxacin in human plas

UPLC法测定儿童血浆中维生素A

目的:临床上建立一种快速、准确测定儿童血浆中维生素A浓度方法.方法:取儿童血浆200μl,加入140μl甲醇和异丙醇(v/v,8:2),涡旋30s后,加入1000μl正已烷,涡旋1min,室温高速离心2min(12000×g),取上清液700μl,吹干后甲醇100μl复溶.色谱条件:色谱柱为BEH C18柱(50mm×2.1mm,1.7μm;Waters公司);流速为0.3ml·min-1;流动相为甲醇-水(90:10);柱温为30℃;进样量:5μL;检测波长为325nm.结果:血浆中维生素A色谱峰分离良好,无干扰,维生素A曲线为y=118296x+11644,R2=0.9997,回收率在90-120%.结论:本法首次使用UPLC法测定血浆中维生素A,且操作简便,适用于儿童血浆中维生素A快速监测.

A sensitive and selective liquid chromatography–tandem mass spectrometric (LC ? MS/MS) method was established to determine 2-oxo-clopidogrel, a crucial intermediate metabolite in human plasma. A chromatographic separation was performed on a Sapphire C18 column following a liquid–liquid extraction sample preparation with methyl t-butyl ether. Detection was carried out on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) with an electrospray ionization (ESI) mode. The method was validated in terms of specificity, accuracy, precision and limit of quantification. The calibration curves ranged from 0.50 to 50.0 ng/mL with good linearity. The stability was fully validated with addition of 1,4-dithio-DL-threitol (DTT) into the plasma sample prior to and in the preparation procedure. The validated method was proved to be suitable for use in pharmacokinetic study after single oral administration of 75 mg clopidogrel tablets in human subjects, which could make contribution to intensive study of the clinical drug–drug interactions of clopidogrel and individual treatment.

A selective, sensitive and high throughput liquid chromatography-tandem mass spectro-metry (LC-ESI-MS/MS) method has been developed for separation and quantification of metoprolol enantiomers on a chiral Lux Amylose-2 (250 mm×4.6 mm, 5 mm) column. Solid phase extraction of (S)-(-)- and (R)-(t)-metoprolol and rac-metoprolol-d6 as an internal standard (IS) was achieved on Lichrosep DVB HL cartridges employing 200 mL human plasma. Both the analytes were chromatographically separated with a resolution factor of 2.24 using 15 mM ammonium acetate in water, pH 5.0 and 0.1% (v/v) diethyl amine in acetonitrile (50:50, v/v) as the mobile phase within 7.0 min. The precursor-product ion transitions for the enantiomers and IS were monitored in the multiple reaction monitoring and positive ionization mode. The method was validated over the concentration range of 0.500-500 ng/mL for both the enantiomers. Matrix effect was assessed by post-column analyte infusion experiment and the mean extraction recovery was greater than 94.0% for both the enantiomers at all quality control levels. The stability of analytes was evaluated in plasma and whole blood under different storage conditions. The method was successfully applied to a clinical study in 14 healthy volunteers after oral administration of 200 mg metoprolol tablet under fasting conditions. The assay reproducibility is shown by reanalysis of 68 incurred samples. The suitability of the developed method was assessed in comparison with different chromatographic methods developed for stereoselective analysis of metoprolol in biological matrices.

A highly sensitive, selective, and precise ultra-performance liquid chromatography tandem mass spectrometry method was developed and validated for simultaneous quantification of itraconazole and hydroxy itraconazole in human plasma by a single liquid-liquid extraction step. The precursor to product ion transitions of m/z 705.3/392.3, m/z 721.2/408.3 and m/z 708.2/435.4 were used to detect and quantify itraconazole, hydroxy itraconazole and itraconazole-d3 respectively. The lower limit of quantitation was found to be 0.500 ng/mL for itraconazole and 1.00 ng/mL for hydroxy itraconazole. The mean recoveries for itraconazole and hydroxy itraconazole were found to be 100.045% and 100.021%, respectively. This developed method with a chromatographic run time of 2.0 min was successfully applied to a bioequivalence study of 100 mg itraconazole capsule.