Faouzi M A, Dine T, Luyckx M, Brunet C, Gressier B, Cazin M, Wallaert B, Cazin J C
Laboratoire de Pharmacologie, Faculté des Sciences Pharmaceutiques et Biologiques, Lille, France.
J Chromatogr B Biomed Appl. 1995 Feb 17;664(2):463-7. doi: 10.1016/0378-4347(94)00473-i.
A simple, sensitive and selective method for the determination of budesonide in bronchoalveolar lavage (BAL) using high-performance liquid chromatography (HPLC) with UV detection was developed. BAL samples were extracted twice with methylene chloride, the extracts were centrifuged and the organic layer separated and dried under nitrogen. The samples were reconstituted in the mobile phase and 80 microliters were injected on to a Spherisorb ODS column with UV absorbance detection at 250 nm. The mobile phase was methanol-aqueous buffer (69:31, v/v). Inter-assay coefficients of variation were measured at 7.81 and 500 ng/ml with ranges of 0.89-7.31%. Average recoveries were 97% or greater. This method was successfully implemented for the analysis of BAL from asthmatics, in order to establish the amount of budesonide available to the lung and to investigate the efficacy of inhaler systems. Patients (n = 9) inhaled four puffs of 200 micrograms of budesonide and BAL was performed 10 min after the last inhalation. Only four BAL out of the nine presented detectable amounts of budesonide. The concentrations in BAL in these four patients were 13.44-84.18 ng/ml, corresponding to total amounts of 0.847-7.997 micrograms.
建立了一种使用高效液相色谱（HPLC）结合紫外检测法测定支气管肺泡灌洗（BAL）中布地奈德的简单、灵敏且选择性高的方法。BAL样本用二氯甲烷萃取两次，萃取液离心，分离有机层并在氮气下干燥。样本用流动相复溶，取80微升注入Spherisorb ODS柱，在250nm处进行紫外吸光度检测。流动相为甲醇 - 水性缓冲液（69:31，v/v）。批间变异系数在7.81和500 ng/ml时测定，范围为0.89 - 7.31%。平均回收率为97%或更高。该方法成功用于分析哮喘患者的BAL，以确定肺部可利用的布地奈德量并研究吸入器系统的疗效。患者（n = 9）吸入4喷200微克的布地奈德，在最后一次吸入后10分钟进行BAL。9份BAL样本中只有4份检测到可检测量的布地奈德。这4名患者BAL中的浓度为13.44 - 84.18 ng/ml，对应总量为0.847 - 7.997微克。
