Analytical methods

分析方法
  • 文章类型: Journal Article
    背景:怀孕期间二手烟(SHS)暴露与不良分娩结局有关,例如低出生体重和早产。虽然问卷通常用于评估SHS暴露,他们捕捉真实曝光的能力可能会有所不同,使研究人员难以协调SHS措施。这项研究旨在将自我报告的SHS暴露与孕妇个人样本中的空气SHS测量结果进行比较。
    方法:SHS是在从204名孕妇收集的48小时综合个人PM2.5Teflon过滤器上测量的,并通过问卷调查获得自我报告的SHS暴露措施。计算了机载SHS测量的描述性统计数据,和方差分析通过自我报告的SHS暴露评估了空气中SHS浓度的组差异。
    结果:参与者为81%的西班牙裔,平均(SD)年龄为28.2(6.0)岁。几何平均(SD)个人空气中SHS浓度为0.14(9.41)µg/m3。报告受教育程度较低的参与者的空中SHS暴露率明显较高(p=0.015)。在报告持续时间较长且家中打开窗户的人中,平均空气中的SHS浓度更高。空气中的SHS和自我报告的SHS暴露之间没有关联;然而,在48小时监测期内询问附近吸烟者的数量与测得的机载SHS最相关(两个以上吸烟者:0.30µg/m3与一个:0.12µg/m3,零:0.15µg/m3;p=0.230)。
    结论:自我报告的SHS暴露与个人PM2.5样本中测得的空气SHS无关。这表明使用SHS问卷进行暴露错误分类,并且需要协调和验证的问题来表征健康研究中的这种暴露。
    结论:这项研究增加了越来越多的证据,表明测量误差是妊娠研究中的主要问题,特别是在依靠自我报告问卷来测量二手烟(SHS)暴露的研究中。该研究介绍了一种使用客观光学测量进行SHS暴露评估的替代方法,这有助于提高暴露评估的准确性。研究结果强调了在妊娠健康研究中使用协调和有效的SHS问卷的重要性,以避免有偏差的效应估计。这项研究可以为未来的研究提供信息,实践,和政策制定,以减少SHS暴露及其对健康的不利影响。
    BACKGROUND: Secondhand smoke (SHS) exposure during pregnancy is linked to adverse birth outcomes, such as low birth weight and preterm birth. While questionnaires are commonly used to assess SHS exposure, their ability to capture true exposure can vary, making it difficult for researchers to harmonize SHS measures. This study aimed to compare self-reported SHS exposure with measurements of airborne SHS in personal samples of pregnant women.
    METHODS: SHS was measured on 48-hour integrated personal PM2.5 Teflon filters collected from 204 pregnant women, and self-reported SHS exposure measures were obtained via questionnaires. Descriptive statistics were calculated for airborne SHS measures, and analysis of variance tests assessed group differences in airborne SHS concentrations by self-reported SHS exposure.
    RESULTS: Participants were 81% Hispanic, with a mean (standard deviation [SD]) age of 28.2 (6.0) years. Geometric mean (SD) personal airborne SHS concentrations were 0.14 (9.41) µg/m3. Participants reporting lower education have significantly higher airborne SHS exposure (p = .015). Mean airborne SHS concentrations were greater in those reporting longer duration with windows open in the home. There was no association between airborne SHS and self-reported SHS exposure; however, asking about the number of smokers nearby in the 48-hour monitoring period was most correlated with measured airborne SHS (Two + smokers: 0.30 µg/m3 vs. One: 0.12 µg/m3 and Zero: 0.15 µg/m3; p = .230).
    CONCLUSIONS: Self-reported SHS exposure was not associated with measured airborne SHS in personal PM2.5 samples. This suggests exposure misclassification using SHS questionnaires and the need for harmonized and validated questions to characterize this exposure in health studies.
    CONCLUSIONS: This study adds to the growing body of evidence that measurement error is a major concern in pregnancy research, particularly in studies that rely on self-report questionnaires to measure SHS exposure. The study introduces an alternative method of SHS exposure assessment using objective optical measurements, which can help improve the accuracy of exposure assessment. The findings emphasize the importance of using harmonized and validated SHS questionnaires in pregnancy health research to avoid biased effect estimates. This study can inform future research, practice, and policy development to reduce SHS exposure and its adverse health effects.
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  • 文章类型: Journal Article
    这篇综述描述了硅(Si)在植物中的作用。还报告了硅的测定和形态形成的方法。植物吸收硅的机制,土壤中的硅组分,概述了动植物在陆地生态系统中Si循环中的参与。考虑了具有不同Si积累能力的豆科植物(尤其是PisumsativumL.和MedicagosativaL.)和禾本科植物(尤其是TriticumaestivumL.),以描述Si在减轻生物和非生物胁迫的负面影响中的作用。本文重点介绍了样品制备,其中包括提取方法和分析技术。已经概述了从植物中分离和表征Si基生物活性化合物的方法。从豌豆中获得的已知生物活性化合物的抗微生物特性和细胞毒性作用,苜蓿,还描述了小麦。
    This review describes the role of silicon (Si) in plants. Methods of silicon determination and speciation are also reported. The mechanisms of Si uptake by plants, silicon fractions in the soil, and the participation of flora and fauna in the Si cycle in terrestrial ecosystems have been overviewed. Plants of Fabaceae (especially Pisum sativum L. and Medicago sativa L.) and Poaceae (particularly Triticum aestivum L.) families with different Si accumulation capabilities were taken into consideration to describe the role of Si in the alleviation of the negative effects of biotic and abiotic stresses. The article focuses on sample preparation, which includes extraction methods and analytical techniques. The methods of isolation and the characterization of the Si-based biologically active compounds from plants have been overviewed. The antimicrobial properties and cytotoxic effects of known bioactive compounds obtained from pea, alfalfa, and wheat were also described.
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  • 文章类型: Journal Article
    The Children\'s Health Exposure Analysis Resource (CHEAR) program allows researchers to expand their research goals by offering the assessment of environmental exposures in their previously collected biospecimens. Samples are analyzed in one of CHEAR\'s network of six laboratory hubs with the ability to assess a wide array of environmental chemicals. The ability to assess inter-study variability is important for researchers who want to combine datasets across studies and laboratories.
    Herein we establish a process of evaluating inter-study variability for a given analytic method.
    Common quality control (QC) pools at two concentration levels (A and B) in urine were created within CHEAR for insertion into each batch of samples tested at a rate of three samples of each pool per 100 study samples. We assessed these QC pool results for seven phthalates analyzed for five CHEAR studies by three different lab hubs utilizing multivariate control charts to identify out-of-control runs or sets of samples associated with a given QC sample. We then tested the conditions that would lead to an out-of-control run by simulating outliers in an otherwise \"in-control\" set of 12 trace elements in blood QC samples (NIST SRM 955c).
    When phthalates were assessed within study, we identified a single out-of-control run for two of the five studies. Combining QC results across lab hubs, all of the runs from these two studies were now in-control, while multiple runs from two other studies were pushed out-of-control. In our simulation study we found that 3-6 analytes with outlier values (5xSD) within a run would push that run out of control in 65-83% of simulations, respectively.
    We show how acceptable bounds of variability can be established for a given analytic method by evaluating QC materials across studies using multivariate control charts.
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  • 文章类型: Journal Article
    Data collected from FDA proficiency tests (PT) during 2012-2018 was used to evaluate the performance of most probable number (MPN) and polymerase chain reaction (PCR) methods used to enumerate Vibrio parahaemolyticus in oyster samples. The primary aim was to establish whether the MPN and PCR methods can be considered equivalent. The following criterion for equivalence was applied: the absolute value of mean bias and between-sample standard deviation must both be less than 0.1 (log10). Final calculations showed mean bias and between-sample standard deviation (SD) were 0.031 and 0.117 (log10) respectively. The between-sample SD criterion was slightly relaxed because with close to 700 results, the data set was large and overall mean bias was low. It was concluded that the two methods can be considered equivalent. The use of PT data for the assessment of method rather than laboratory performance is a secondary topic addressed in this paper. Important requirements for this use of PT data include availability of sufficient results for both methods and use of real food matrices. Ultimately, the results presented here provide an example of how PT data can be used to monitor method performance across many laboratories and samples as well as to assess method equivalence.
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  • 文章类型: Case Reports
    The rapid development of fluorescent probes for monitoring target enzymes is still a great challenge owing to the lack of efficient ways to optimize a specific fluorophore. Herein, a practical two-dimensional strategy was designed for the development of an isoform-specific probe for CYP3A4, a key cytochrome P450 isoform responsible for the oxidation of most clinical drugs. In first dimension of the design strategy, a potential two-photon fluorescent substrate (NN) for CYP3A4 was effectively selected using ensemble-based virtual screening. In the second dimension, various substituent groups were introduced into NN to optimize the isoform-selectivity and reactivity. Finally, with ideal selectivity and sensitivity, NEN was successfully applied to the real-time detection of CYP3A4 in living cells and zebrafish. These findings suggested that our strategy is practical for developing an isoform-specific probe for a target enzyme.
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  • Unknown products identified precisely: The coupling of liquid chromatography to NMR spectroscopy, mass spectrometry, and infrared spectroscopy and the use of high-resolution mass spectrometry is utilized to investigate the formation of atmospheric-relevant organic aerosols. The investigation focussed on the gas-phase reaction of α-pinene with ozone and the subsequent identification of the reaction products by the coupled analytical techniques.
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  • 文章类型: Comparative Study
    Among the biological markers of morbidity and mortality, albumin holds a key place in the range of criteria used by the High Authority for Health (HAS) for the assessment of malnutrition and the coding of information system medicalization program (PMSI). If the principle of quantification methods have not changed in recent years, the dispersion of external evaluations of the quality (EEQ) data shows that the standardization using the certified reference material (CRM) 470 is not optimal. The aim of this multicenter study involving 7 sites, conducted by a working group of the French Society of Clinical Biology (SFBC), was to assess whether the albuminemia values depend on the analytical system used. The albumin from plasma (n=30) and serum (n=8) pools was quantified by 5 different methods [bromocresol green (VBC) and bromocresol purple (PBC) colorimetry, immunoturbidimetry (IT), immunonephelometry (IN) and capillary electrophoresis (CE)] using 12 analyzers. Bland and Altman\'s test evaluated the difference between the results obtained by the different methods. For example, a difference as high as 13 g/L was observed for the same sample between the methods (p <0.001) in the concentration range of 30 to 35 g/L. The VBC overestimates albumin across the range of values tested compared to PBC (p <0.05). PBC method gives similar results to IN for values lower than 40 g/L. For IT methods, one of the technical/analyzer tandem underestimates the albumin values inducing a difference of performance between the immunoprecipitation methods (IT vs IN, p <0.05). Although, the albumin results are related to the technical/analyzer tandem used. This variability is usually not taken into account by the clinician. Thus, clinicians and biologists have to be aware and have to check, depending on the method used, the albumin thresholds identified as risk factors for complications related to malnutrition and PMSI coding.
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  • 文章类型: Journal Article
    An efficient and robust method to measure vitamin D (25-hydroxy vitamin D3 (25(OH)D3) and 25-hydroxy vitamin D2 in dried blood spots (DBS) has been developed and applied in the pan-European multi-centre, internet-based, personalised nutrition intervention study Food4Me. The method includes calibration with blood containing endogenous 25(OH)D3, spotted as DBS and corrected for haematocrit content. The methodology was validated following international standards. The performance characteristics did not reach those of the current gold standard liquid chromatography-MS/MS in plasma for all parameters, but were found to be very suitable for status-level determination under field conditions. DBS sample quality was very high, and 3778 measurements of 25(OH)D3 were obtained from 1465 participants. The study centre and the season within the study centre were very good predictors of 25(OH)D3 levels (P<0·001 for each case). Seasonal effects were modelled by fitting a sine function with a minimum 25(OH)D3 level on 20 January and a maximum on 21 July. The seasonal amplitude varied from centre to centre. The largest difference between winter and summer levels was found in Germany and the smallest in Poland. The model was cross-validated to determine the consistency of the predictions and the performance of the DBS method. The Pearson\'s correlation between the measured values and the predicted values was r 0·65, and the sd of their differences was 21·2 nmol/l. This includes the analytical variation and the biological variation within subjects. Overall, DBS obtained by unsupervised sampling of the participants at home was a viable methodology for obtaining vitamin D status information in a large nutritional study.
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  • 文章类型: Comparative Study
    We describe here a systematic, reliable, and fast screening method that allows the comparison of H2-forming catalysts that work under aqueous conditions with two readily prepared chemical reductants and two commonly used photosensitizers. This method uses a Clark-type microsensor for H2 detection and complements previous methods based on rotating disk electrode measurements. The efficiencies of a series of H2 -producing catalysts based on Co, Ni, Fe, and Pt were investigated in aqueous solutions under thermal conditions with europium(II) reductants and under photochemical conditions in the presence of two different photosensitizers {[Ru(bipy)3]Cl2(bipy=2,2-bipyridine) and eosin-Y} and sacrificial electron donors (ascorbate and triethanolamine, respectively). The majority of catalysts tested were active only under specific conditions. However, our results also demonstrate the impressive versatility of a group of Co catalysts, which were able to produce H2 under different reducing conditions and at various pH values. In particular, a cobaloxime, [Co(dmgH)2(H2O)2] (dmgH2 =dimethylglyoxime), and a cobalt tetraazamacrocyclic complex, {Co(CR)Cl2}(+) [CR=2,12-dimethyl-3,7,11,17-tetraazabicylo(11.3.1)heptadeca-1(17),2,11,13,15-pentaene], displayed excellent catalytic rates under the studied conditions, and the best rates were observed under thermal conditions.
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  • 文章类型: Comparative Study
    OBJECTIVE: To examine if fasting affects serum bilirubin levels in clinically healthy males and females.
    METHODS: We used retrospective data from phase I clinical trials where blood was collected in either a fed or fasting state at screening and predosing time points and analysed for total bilirubin levels as per standard clinical procedures. Participants were clinically healthy males (n=105) or females (n=30) aged 18-48 inclusive who participated in a phase I clinical trial in 2012 or 2013.
    RESULTS: We found a statistically significant increase in total serum bilirubin levels in fasting males as compared with non-fasting males. The fasting time correlated positively with increased bilirubin levels. The age of the healthy males did not correlate with their fasting bilirubin level. We found no correlation between fasting and bilirubin levels in clinically normal females.
    CONCLUSIONS: The recruitment and screening of volunteers for a clinical trial is a time-consuming and expensive process. This study clearly demonstrates that testing for serum bilirubin should be conducted on non-fasting male subjects. If fasting is required, then participants should not be excluded from a trial based on an elevated serum bilirubin that is deemed non-clinically significant.
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