摘要
目的:对人粪便中匹诺塞林浓度的高效液相色谱质谱联用(LC-MS/MS)定量分析方法的测量不确定度进行评定。方法:分析人粪便中匹诺塞林浓度测定过程,确定并简化不确定度来源,利用LC-MS/MS测定人粪便中匹诺塞林的方法学验证数据,通过统计学方法,依次计算各变量的不确定度、合成不确定度和扩展不确定度。结果:人粪便中低(51.07 ng·mL-1)、中(510.44ng·mL-1)和高(2957.50 ng·mL-1)质量浓度匹诺塞林的扩展不确定度分别为14.58 ng·mL-1、26.30ng·mL-1和206.46 ng·mL-1(k=2,置信概率为95%)。结论:测量不确定度与检测结果数值相关,随浓度高低不同而有所差异,而且测定不确定度比例在匹诺塞林不同浓度的结果也不相同,标准曲线拟合对低浓度点的影响非常大。
Objective： To set out the procedures for evaluation of measurement uncertainty for the determination of pinocembrin in human feces by high-performance liquid chromatography-tandem mass spectrometry. Methods： Detection process was analyzed. Uncertainty sources were established and simplified, then calculated each component of uncertainty, combined uncertainty and expanded uncertainty. Results： The expand uncertainty of pinocembrin with low （51.07 ng·mL-1）, medium （510.44 ng·mL-1） and high）2957.50 ng·mL-1）concentration was 14.58 ng·mL-1, 26.30 ng·mL-1 and 206.46 ng·mL-1, respectively （k=2,conifdence probability was 95%）. Conclusions： Uncertainty for the determination of pinocembrin in human feces was related to the detecting data, and the proportion of uncertainty was different in low, medium and high concentration. The standard curve iftting had a great inlfuence on the uncertainty at the low level of pinocembrin.
出处
《临床药物治疗杂志》
2014年第2期35-39,共5页
Clinical Medication Journal
基金
国家科技部"重大新药创制"科技重大专项心脑血管疾病新药临床评价技术平台研究(2012ZX09303008-002)
国家自然科学基金(81202601)
关键词
匹诺塞林
粪便
不确定度
LC-MS/MS
LC-MS/MS
Pinocembrin
Feces
Uncertainty
