Wilson N D, Watt R A, Moffat A C
Centre for Pharmaceutical Analysis, The School of Pharmacy, University of London, UK.
J Pharm Pharmacol. 2001 Jan;53(1):95-102. doi: 10.1211/0022357011775064.
Thirty different eucalyptus oil samples were scanned on the FOSS NIRSystems 6500 Rapid Content Sampler using a reflectance vessel as sample presentation method. The cineole content of each sample was determined by the BP method and these reference data were used to construct two calibration equations for cineole content in the oils using Vision software. The mean accuracy for the NIR method differed by 1.01% or less, and the mean bias by +/-0.33% or less, compared with the BP method. Calculation of the 95% confidence intervals for the slope and intercept of plots of NIR predicted values against BP method reference values showed that there was no evidence of fixed or relative systematic errors. Tests for short-term and intermediate repeatability were conducted. The standard deviation was 0.83% w/w or less and the coefficient of variation was 1.11% or less. The confidence intervals for both short-term and intermediate repeatability overlapped with that for the BP method, suggesting that there was no evidence for a difference in values obtained by the BP and NIR methods. The range of cineole contents used in the calibrations was extended by incorporating five samples of eucalyptus oil spiked with cineole, and five samples of two essential oils known to have a lower cineole content than eucalyptus oil, to give a range of 52.5 to 99.0% w/w. The mean accuracy decreased to an error of 1.26% or less and the bias to +/-0.50% or less. Again, confidence intervals suggested there was no evidence for fixed or systematic errors in the NIR calibrations. We propose that NIR spectroscopy could be used as an alternative method for the determination of cineole content in eucalyptus oils.
使用反射容器作为样品呈现方法,在FOSS NIRSystems 6500快速含量采样仪上对30个不同的桉叶油样品进行扫描。通过英国药典(BP)方法测定每个样品的桉叶油素含量,并使用Vision软件将这些参考数据用于构建两个关于桉叶油中桉叶油素含量的校准方程。与BP方法相比,近红外(NIR)方法的平均准确度差异在1.01%或更低,平均偏差在±0.33%或更低。计算NIR预测值与BP方法参考值的斜率和截距的95%置信区间,结果表明没有固定或相对系统误差的证据。进行了短期和中期重复性测试。标准偏差为0.83%(w/w)或更低,变异系数为1.11%或更低。短期和中期重复性的置信区间与BP方法的置信区间重叠,这表明没有证据表明BP方法和NIR方法获得的值存在差异。通过加入五个添加了桉叶油素的桉叶油样品以及五个已知桉叶油素含量低于桉叶油的两种精油样品,扩展了校准中使用的桉叶油素含量范围,使其达到52.5%至99.0%(w/w)。平均准确度降至误差1.26%或更低,偏差降至±0.50%或更低。同样,置信区间表明没有证据表明NIR校准存在固定或系统误差。我们建议NIR光谱法可作为测定桉叶油中桉叶油素含量的替代方法