气相色谱法测定丁香酚含量的测量不确定度评定

IF 1 4区 工程技术 Q4 CHEMISTRY, ANALYTICAL
Dalin Chann, Sophany Ret, Chun Li, Xinxin Ding, Meng Liang
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引用次数: 0

摘要

丁香(Syzygium aromaticum)因其高丁香酚含量而受到重视,需要精确定量以进行质量控制。本研究以水杨酸甲酯为内标,按照中国药典2015年的方法,采用气相色谱-火焰电离检测法测定商业丁香样品中的丁香酚。根据《测量不确定度表达指南》和EURACHEM/CITAC指南,对与该测定相关的测量不确定度进行了综合评估。确定并量化了主要潜在不确定度来源,包括相对校正因子、峰面积(分析物和内标物)、样品量、内标物浓度、样品质量和可重复性。丁香酚的平均含量为17.91% m/m。丁香酚含量符合《中国药典》要求的阈值(不低于11.0% m/m),确认该商品适合药用。计算出组合相对标准不确定度为0.199,扩展不确定度为7.12%(覆盖因子k = 2),对应于丁香酚含量的绝对不确定度为±1.28% m/m(或±12.8 mg/g)。总体不确定度的主要影响因素被确定为内部标准的峰面积和方法的可重复性,在确定的不确定度范围内验证方法的质量控制可靠性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Evaluating the measurement uncertainty in determination of eugenol content in cloves by gas chromatography

Evaluating the measurement uncertainty in determination of eugenol content in cloves by gas chromatography

Evaluating the measurement uncertainty in determination of eugenol content in cloves by gas chromatography

Cloves (Syzygium aromaticum) are valued for their high eugenol content, necessitating accurate quantification for quality control. This study determined eugenol in a commercial clove sample using Gas Chromatography with Flame Ionization Detection, employing methyl salicylate as an internal standard following the Chinese Pharmacopoeia 2015 methodology. A comprehensive evaluation of the measurement uncertainty associated with this determination was performed according to the Guide to the Expression of Uncertainty in Measurement and EURACHEM/CITAC guidelines. Major potential uncertainty sources, including the relative correction factor, peak areas (analyte and internal standard), sample volume, internal standard concentration, sample mass, and repeatability, were identified and quantified. The average eugenol content was found to be 17.91% m/m. The eugenol content met the threshold required by the Chinese Pharmacopoeia (which mandates not less than 11.0% m/m) and confirmed the suitability of the commercial product for medicinal use. The combined relative standard uncertainty was calculated as 0.199, leading to an expanded uncertainty of 7.12% (coverage factor k = 2), corresponding to an absolute uncertainty of ± 1.28% m/m eugenol content (or ± 12.8 mg/g). The primary contributors to the overall uncertainty were identified as the peak area of the internal standard and method repeatability, validating the method's reliability for quality control purposes within the established uncertainty limits.

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来源期刊
Accreditation and Quality Assurance
Accreditation and Quality Assurance 工程技术-分析化学
CiteScore
1.80
自引率
22.20%
发文量
39
审稿时长
6-12 weeks
期刊介绍: Accreditation and Quality Assurance has established itself as the leading information and discussion forum for all aspects relevant to quality, transparency and reliability of measurement results in chemical and biological sciences. The journal serves the information needs of researchers, practitioners and decision makers dealing with quality assurance and quality management, including the development and application of metrological principles and concepts such as traceability or measurement uncertainty in the following fields: environment, nutrition, consumer protection, geology, metallurgy, pharmacy, forensics, clinical chemistry and laboratory medicine, and microbiology.
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