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LCMSMS法测动物源食品中硝呋烯腙残留量的不确定度评定 被引量:2
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作者 罗艳霞 《广州化工》 CAS 2016年第13期136-139,173,共5页
建立了液相色谱-串联质谱测定动物源食品硝呋烯腙的方法,并对其不确定度进行了评定。本文研究了液相色谱-串联质谱测定动物源食品硝呋烯腙含量的方法,并依据CNAS-GL06-2006《化学分析中不确定度的评估指南》和JJF1059.1-2012《测量不确... 建立了液相色谱-串联质谱测定动物源食品硝呋烯腙的方法,并对其不确定度进行了评定。本文研究了液相色谱-串联质谱测定动物源食品硝呋烯腙含量的方法,并依据CNAS-GL06-2006《化学分析中不确定度的评估指南》和JJF1059.1-2012《测量不确定度评定与表示》规定的原理与方法,分析了实验过程中不确定性的来源,建立了不确定度评定的数学模型,计算并分析了合成不确定度的结果。由结果可知:在液相色谱-串联质谱测定动物源食品硝呋烯腙含量过程中,校准曲线拟合与标准溶液的配置是影响其不确定度的主要因素,液相色谱-串联质谱仪和测量重复性是次要因素。 展开更多
关键词 lcmsms 动物源性食品 硝呋烯腙 不确定度
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Method Development for the Detection of Basic/Weak Basic Drugs in Hair by LCMSMS: Comparison between Methanolic and Alkaline Extraction on Real Samples 被引量:1
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作者 Jaber Al Jaber David Holt Atholl Johnston 《Pharmacology & Pharmacy》 2012年第3期263-274,共12页
Detection of drugs in hair has become popular in recent years. The significantly long drug detection window (months) in hair has allowed the retrospective investigation and measurement of past consumption of drug. As ... Detection of drugs in hair has become popular in recent years. The significantly long drug detection window (months) in hair has allowed the retrospective investigation and measurement of past consumption of drug. As the majority of drugs are basic, an extraction method was developed based on a methanolic solution for detection of basic/weak basic drugs in hair. It was compared with alkaline digestion (NaOH) followed by LLE. A filtration step with filtration vials was added and their materials were compared. After filtration, extracts were injected directly onto a C18 column coupled to Sciex ABI 2000 MSMS. The mobile phase was 50% methanol, 0.1% formic acid and 2 mM ammonium acetate (isocratic). Both methods were compared by applying them to real samples. Results showed that calibration was linear with r2 of 0.991-0.999 for 20 tested analytes. The matrix effect was assessed to be between 91.4%- 110.2% for 18 analytes. PTFE filter material showed better recoveries over the GMF and PVDF based filters. Stability of analytes during extraction in general was better with methanolic incubation rather than alkaline digestion. With regard to real sample recovery, 6 out of 10 analytes recovered better with alkaline digestion. In conclusion, the methanolic method is capable of extracting most basic drugs in hair samples but only part of the total incorporated drug. Therefore, these results suggest that a combination of both methods (methanolic and alkaline extractions) in hair sample processing for general detection of basic and weak basic drugs may produce better results. However, not all basic drugs are stable under alkaline digestion. 展开更多
关键词 HAIR Analysis Basic DRUGS lcmsms BENZODIAZEPINES Method Development LLE
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