海水中兽药多残留分析时，基质效应会对测定准确度产生较大影响．以反渗透水为空白对照，液相色谱-串联质谱联用（1iquid chromatography-tandem mass spectrometry，LC—MS／Ms）检测，在500倍浓缩条件下，评价了3种常用亲水一亲油平衡...海水中兽药多残留分析时，基质效应会对测定准确度产生较大影响．以反渗透水为空白对照，液相色谱-串联质谱联用（1iquid chromatography-tandem mass spectrometry，LC—MS／Ms）检测，在500倍浓缩条件下，评价了3种常用亲水一亲油平衡（hydrophile-lyophile balance，HLB）固相萃取柱（Waters、Supelco和安谱）对海水中35种兽药的基质效应和保留效果．研究发现：反渗透水实验中3种HLB柱表现出柱填料的外源性基质效应，喹诺酮类和四环素类兽药呈现基质正效应，雌激素类等呈现基质负效应，磺胺类和氯霉素类兽药基质效应不显著．海水基质实验中由于外源性杂质与内源性杂质共同作用，大部分喹诺酮类和四环素类兽药呈现基质正效应，氯霉素类和雌激素类呈现基质负效应，磺胺类兽药基质效应不显著．与外标法相比较，基质匹配标准校正法可有效消除基质效应．在50和200ng／L两个加标质量浓度下，3种HLB柱对海水中35种目标兽药校正后的回收率分别为26．8％～147．8％（Waters）、60．4％～159．3％（Supelco）和52．0％～112．1％（安谱）；两个加标浓度的相对标准偏差（RSD）（n=4）在0．1％～11．1％．结果表明，相同实验条件下，3种HLB柱的基质效应不容忽视，采用基质匹配标准校正法可以有效克服基质效应，为海水样品中兽药多残留分析方法准确度的改善提供了参考数据．展开更多
Measurement uncertainty plays an important role in laser tracking measurement analyses. In the present work, the guides to the expression of uncertainty in measurement(GUM) uncertainty framework(GUF) and its supplemen...Measurement uncertainty plays an important role in laser tracking measurement analyses. In the present work, the guides to the expression of uncertainty in measurement(GUM) uncertainty framework(GUF) and its supplement, the Monte Carlo method, were used to estimate the uncertainty of task-specific laser tracker measurements. First, the sources of error in laser tracker measurement were analyzed in detail, including instruments, measuring network fusion, measurement strategies, measurement process factors(such as the operator), measurement environment, and task-specific data processing. Second, the GUM and Monte Carlo methods and their application to laser tracker measurement were presented. Finally, a case study involving the uncertainty estimation of a cylindricity measurement process using the GUF and Monte Carlo methods was illustrated. The expanded uncertainty results(at 95% confidence levels) obtained with the Monte Carlo method are 0.069 mm(least-squares criterion) and 0.062 mm(minimum zone criterion), respectively, while with the GUM uncertainty framework, none but the result of least-squares criterion can be got, which is 0.071 mm. Thus, the GUM uncertainty framework slightly underestimates the overall uncertainty by 10%. The results demonstrate that the two methods have different characteristics in task-specific uncertainty evaluations of laser tracker measurements. The results indicate that the Monte Carlo method is a practical tool for applying the principle of propagation of distributions and does not depend on the assumptions and limitations required by the law of propagation of uncertainties(GUF). These features of the Monte Carlo method reduce the risk of an unreliable measurement of uncertainty estimation, particularly in cases of complicated measurement models, without the need to evaluate partial derivatives. In addition, the impact of sampling strategy and evaluation method on the uncertainty of the measurement results can also be taken into account with Monte Carlo method, which plays a guiding role in measurement planning.展开更多
文摘海水中兽药多残留分析时，基质效应会对测定准确度产生较大影响．以反渗透水为空白对照，液相色谱-串联质谱联用（1iquid chromatography-tandem mass spectrometry，LC—MS／Ms）检测，在500倍浓缩条件下，评价了3种常用亲水一亲油平衡（hydrophile-lyophile balance，HLB）固相萃取柱（Waters、Supelco和安谱）对海水中35种兽药的基质效应和保留效果．研究发现：反渗透水实验中3种HLB柱表现出柱填料的外源性基质效应，喹诺酮类和四环素类兽药呈现基质正效应，雌激素类等呈现基质负效应，磺胺类和氯霉素类兽药基质效应不显著．海水基质实验中由于外源性杂质与内源性杂质共同作用，大部分喹诺酮类和四环素类兽药呈现基质正效应，氯霉素类和雌激素类呈现基质负效应，磺胺类兽药基质效应不显著．与外标法相比较，基质匹配标准校正法可有效消除基质效应．在50和200ng／L两个加标质量浓度下，3种HLB柱对海水中35种目标兽药校正后的回收率分别为26．8％～147．8％（Waters）、60．4％～159．3％（Supelco）和52．0％～112．1％（安谱）；两个加标浓度的相对标准偏差（RSD）（n=4）在0．1％～11．1％．结果表明，相同实验条件下，3种HLB柱的基质效应不容忽视，采用基质匹配标准校正法可以有效克服基质效应，为海水样品中兽药多残留分析方法准确度的改善提供了参考数据．
基金Project(51318010402)supported by General Armament Department Pre-Research Program of China
文摘Measurement uncertainty plays an important role in laser tracking measurement analyses. In the present work, the guides to the expression of uncertainty in measurement(GUM) uncertainty framework(GUF) and its supplement, the Monte Carlo method, were used to estimate the uncertainty of task-specific laser tracker measurements. First, the sources of error in laser tracker measurement were analyzed in detail, including instruments, measuring network fusion, measurement strategies, measurement process factors(such as the operator), measurement environment, and task-specific data processing. Second, the GUM and Monte Carlo methods and their application to laser tracker measurement were presented. Finally, a case study involving the uncertainty estimation of a cylindricity measurement process using the GUF and Monte Carlo methods was illustrated. The expanded uncertainty results(at 95% confidence levels) obtained with the Monte Carlo method are 0.069 mm(least-squares criterion) and 0.062 mm(minimum zone criterion), respectively, while with the GUM uncertainty framework, none but the result of least-squares criterion can be got, which is 0.071 mm. Thus, the GUM uncertainty framework slightly underestimates the overall uncertainty by 10%. The results demonstrate that the two methods have different characteristics in task-specific uncertainty evaluations of laser tracker measurements. The results indicate that the Monte Carlo method is a practical tool for applying the principle of propagation of distributions and does not depend on the assumptions and limitations required by the law of propagation of uncertainties(GUF). These features of the Monte Carlo method reduce the risk of an unreliable measurement of uncertainty estimation, particularly in cases of complicated measurement models, without the need to evaluate partial derivatives. In addition, the impact of sampling strategy and evaluation method on the uncertainty of the measurement results can also be taken into account with Monte Carlo method, which plays a guiding role in measurement planning.
