Determination of camphor and menthol in compound camphor liniment by GC and evaluation of uncertainty
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摘要: 目的 建立测定复方樟脑搽剂中主要成分樟脑和薄荷脑含量的气相色谱（GC）法，并探讨不确定度评估方法。 方法 采用GC法，以萘为内标物，Thermo TG-WAXMS毛细管柱（30.0 m×0.25 mm，涂层厚0.5 μm），FID检测器；分析测量过程不确定度的来源，建立数学模型，计算合成标准不确定度和扩展不确定度。 结果 樟脑和薄荷脑分别在8.56~85.6μg/ml、11.2~112.0 μg/ml质量浓度范围内线性关系良好，樟脑平均加样回收率100.20%、RSD为0.892%（n=9），薄荷脑平均加样回收率99.65%、RSD为1.369%（n=9）；扩展不确定度分别为0.630 mg/ml （k=2）、0.656 mg/ml （k=2），樟脑含量为（20.74±0.630） mg/ml、薄荷脑含量为（20.48±0.656） mg/ml。 结论 气相色谱方法准确、灵敏、重现性好，可用于复方樟脑搽剂中樟脑和薄荷脑含量测定；不确定度评定有利于进一步提高含量测定的准确性。Abstract: Objective To establish a gas chromatography (GC) method to determine the contents of camphor and menthol in compound camphor liniment and to evaluate the uncertainty. Methods Thermo TG-WAXMS (30.0 m×0.25 mm, 0.5 μm) and FID were used with naphtalinas as internal standard. The uncertainty sources of measurement were analyzed and a mathematical model was established to calculate the combined standard uncertainty and the expanded uncertainty. Results A good linear relationship was observed in the concentration range of 8.56-85.6μg/ml for camphor and 11.2-112.0 μg/ml for menthol, the average recoveries were 100.20% and 99.65% with RSD 0.892% and 1.369% (n=9). The expanded uncertainty U95 were 0.630 mg/ml (k=2), 0.656 mg/ml (k=2), The content of camphor was (20.74±0.602) mg/ml and menthol was (20.48±1.336) mg/ml. Conclusion The method is accurate, sensitive. It has good repeatability for controlling the quality of camphor and menthol in compound camphor liniment. The mathematic model of uncertainty can be used to improve the assay accuracy.
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Key words:
- GC /
- compound camphor liniment /
- content determination /
- measurement uncertainty
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