Mennickent Sigrid, Fierro Ricardo, Vega Mario, de Diego Marta, Godoy C Gloria
Department of Pharmacy, Faculty of Pharmacy, University of Concepción, Concepción, Chile.
J Sep Sci. 2009 May;32(9):1454-8. doi: 10.1002/jssc.200800675.
An instrumental planar chromatographic (HPTLC) method for quantification of carbamazepine in human serum was developed using liquid-liquid extraction with dichloromethane, fluorescence activation with perchloric acid 60%/ethanol/water (1:1:1, v/v) and fluorescence detection. Planar chromatographic separation was performed on precoated silica gel F254 HPTLC plates using a mixture of ethyl acetate/toluene/methanol/acetic acid glacial (5:4:0.5:0.5, v/v) as mobile phase. Densitometric detection was done at 366 nm. The method was validated for linearity, precision and accuracy. Linear calibration curves in the range of 3 and 20 ng/microL showed correlation coefficient of 0.998. The intra-assay and inter-assay precision, expressed as the RSD, were in the range of 0.41-1.24% (n = 3) and 2.17-3.17% (n = 9), respectively. The LOD was 0.19 ng, and the LOQ was 0.57 ng. Accuracy, calculated as percentage recovery, was between 98.98 and 101.96%, with a RSD not higher than 1.52%. The method was selective for the active principle tested. In conclusion, the method is useful for quantitative determination of carbamazepine in human serum.
建立了一种用于定量测定人血清中卡马西平的仪器平面色谱法(高效薄层色谱法),该方法采用二氯甲烷液 - 液萃取、60%高氯酸/乙醇/水(1:1:1,v/v)荧光活化及荧光检测。平面色谱分离在预涂硅胶F254高效薄层色谱板上进行,以乙酸乙酯/甲苯/甲醇/冰醋酸(5:4:0.5:0.5,v/v)的混合物作为流动相。在366 nm处进行光密度检测。该方法在线性、精密度和准确度方面得到了验证。3至20 ng/μL范围内的线性校准曲线显示相关系数为0.998。批内和批间精密度,以相对标准偏差(RSD)表示,分别在0.41 - 1.24%(n = 3)和2.17 - 3.17%(n = 9)范围内。检测限为0.19 ng,定量限为0.57 ng。以回收率百分比计算的准确度在98.98%至101.96%之间,相对标准偏差不高于1.52%。该方法对所检测的活性成分具有选择性。总之,该方法可用于人血清中卡马西平的定量测定。