Mandel’s Test: A Case of Oversimplification?

Polly-Anna Ashford is a guest web writer for Analytical Methods. She is currently a PhD student at the University of East Anglia, UK.

Mandel's test for goodness of fit

The economic and time constraints that limit the collection of calibration data mean that analytical chemists rely on robust statistical tests for linearity to support the accuracy of their findings. Mandel’s test was first proposed in 1964 and despite being simplified and suggested by IUPAC in 1998, has not been used broadly. Recently the Mandel’s test enjoyed an increase in popularity, possibly because non-linear data points are now more straightforward to plot using spreadsheets (linear model).

In this Analytical Methods paper, José M. Andrade and María P. Gómez-Carracedo at the University of A Coruna examined the validity of the definition of the test provided by IUPAC. They compared this approach to Mandel’s original definition, presenting ten different scenarios from simulated data. These simulations vary by number of data points and magnitude of the variances of the linear (IUPAC) or non-linear (Mandel’s) models. Surprisingly, the authors concluded that the 1998 IUPAC interpretation of this test does not strictly adhere to the definition published by Mandel, and is only valid within certain key limitations. The authors provide useful recommendations to analytical chemists intending to use Mandel’s test in their calibration calculations.

Notes on the use of Mandel’s test to check for nonlinearity in laboratory calibrations
J. M. Andrade and M. P. Gómez-Carracedo
Anal. Methods, 2013, Advance Article
DOI: 10.1039/C2AY26400E

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Analytical Methods Issue 3 NOW online!

Kiefer and Kaspereit, Anal. Methods, 2013, 5, 797-800

Here we go with the third issue of Analytical Methods now online!  If you are interested in the most recent analytical developments, take a look at the latest papers we have just published.

First, here are the two covers of the issue for you to enjoy. The outside front cover shows an image featuring the work of Johannes Kiefer and his group from the University of Erlangen-Nuremberg, Germany. The team introduced a new Raman set-up taking into account the optical activity and improved the interpretation of spectroscopic data by determining the depolarization ratio in optically active samples.

Determination of the Raman depolarization ratio in optically active samples
Johannes Kiefer and Malte Kaspereit
Anal. Methods, 2013,5, 797-800
DOI: 10.1039/C2AY25987G

Huck-Pezzei et al., Anal. Methods, 2013, 5, 616-628

The lively inside front cover of this issue is a colourful snapshot of a study coming from Austria. Christian Huck and co-workers present a novel analytical platform that enables analysis of St John’s wort extracts and tissue. The researchers show a fast and non-destructive quantitation and quality control to identify adulterations which are usually hard to identify.

A chromatographic and spectroscopic analytical platform for the characterization of St John’s wort extract adulterations
V. A. Huck-Pezzei ,  L. K. Bittner ,  J. D. Pallua ,  H. Sonderegger ,  G. Abel ,  M. Popp ,  G. K. Bonn and C. W. Huck
Anal. Methods, 2013,5, 616-628
DOI: 10.1039/C2AY26030A

Along with the covers of Issue 3, here is an informative Critical Review written by Antonio Rangel and colleagues. The authors explain how the sequential injection lab-on-valve platform has proven to be a powerful tool in the automation of solid phase extraction. To read the full article, please access the link below:

Scheme of a sequential injection lab-on-valve platform

Sequential injection lab-on-valve platform as a miniaturisation tool for solid phase extraction
Susana S. M. P. Vidigal ,  Ildikó V. Tóth and António O. S. S. Rangel
Anal. Methods, 2013,5, 585-597
DOI: 10.1039/C2AY26322J

In addition, here are some HOT papers free for you to read until February 1st. Have a read now!

The feasibility of wavelength dispersive X-ray fluorescence spectrometry for the assessment of lead concentration in animal bone powder
José A. A. Brito ,  Inês I. B. Cavaleiro ,  Tânia A. P. Fernandes and Luísa M. L. Gonçalves
Anal. Methods, 2013,5, 598-602
DOI: 10.1039/C2AY26455B

Metal enhanced fluorescent biosensing assays for DNA through the coupling of silver nanoparticles
Weibing Qiang ,  Hui Li and Danke Xu
Anal. Methods, 2013,5, 629-635
DOI: 10.1039/C2AY26097B

Obelin mutants as reporters in bioluminescent dual-analyte binding assay
Vasilisa V. Krasitskaya ,  Alexander N. Kudryavtsev ,  Osamu Shimomura and Ludmila A. Frank
Anal. Methods, 2013,5, 636-640
DOI: 10.1039/C2AY25976A

ZnAl2O4-based luminescent marker for gunshot residue identification and ammunition traceability
M. A. Melo Lucena ,  G. F. de Sá ,  M. O. Rodrigues ,  S. Alves ,  M. Talhavini and I. T. Weber
Anal. Methods, 2013,5, 705-709
DOI: 10.1039/C2AY25535A

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A new graphite sensor for detection of selenium

Detection of selenium using graphite-based sensors

Researchers from the Manchester Metropolitan University reported the first example of graphite-based sensors to detect selenium in drinking water.
Selenium is a trace mineral nutrient essential as for all animals, but it is extremely toxic if the intake dose exceeds 400 µg per day. Both the European Union and United States Environmental Protection Agency (EPA) have set the limits for selenium in drinking water to of 10 µg/L and 50 µg/L respectively.

Today, the gold-based electrodes which are traditionally used to detect selenium are very expensive. With this work, Craig Banks and his group address the problem proposing a graphite based sensor to detect selenium in water. They fabricated special screen-printed graphite electrodes and detected low concentrations of selenium in their laboratory tap water, with a limit of detection which fell below those set by the EPA. According to the authors, this new graphite-based sensor could represent an appealing alternative to the gold based electrodes currently used.

To know more about this work, click on the link below. This paper will be free to read until January 24th.

Electroanalytical sensing of selenium(IV) utilising screen printed graphite macro electrodes
Athanasios V. Kolliopoulos ,  Jonathan P. Metters and Craig E. Banks
Anal. Methods, 2013, Advance Article
DOI: 10.1039/C2AY26041G

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HOT articles in Analytical Methods

Take a look at the new detection methods described in these HOT articles in Analytical Methods! They include detection of medicinal products such as ginseng using near infrared spectral fingerprints and determination of lead in animal bone powder by X-ray fluorescence spectroscopy. These papers will be free to read until January 24th.

Expeditious identification and semi-quantification of Panax ginseng using near infrared spectral fingerprints and multivariate analysis
Juan Ricardo Lucio-Gutiérrez ,  Jordi Coello and S Maspoch
Anal. Methods, 2012, Accepted Manuscript
DOI: 10.1039/C2AY26235E

The feasibility of wavelength dispersive X-ray fluorescence spectrometry for the assessment of lead concentration in animal bone powder
José A. A. Brito ,  Inês I. B. Cavaleiro ,  Tânia A. P. Fernandes and Luísa M. L. Gonçalves
Anal. Methods, 2013, Advance Article
DOI: 10.1039/C2AY26455B

Determination of lead in animal bone powder

More articles for you to enjoy:

Novel pH sensor based on anthraquinone–ferrocene modified free standing gold nanowire array electrode
Louise Devlin ,  Mamun Jamal and Kafil Mahmood Razeeb
Anal. Methods, 2012, Accepted Manuscript
DOI: 10.1039/C2AY26264A

Combining enzymatic 18O-labeling and 2-D LC-MS/MS for study of protein interactions in primary T cells
Diana Lang ,  Sabine Anker ,  Benno Kuropka and Eberhard Krause
Anal. Methods, 2012, Accepted Manuscript
DOI: 10.1039/C2AY26298C

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A Novel Eu-POM Sensor for Nitrite, Iodate and Bromate Detection

Polly-Anna Ashford is a guest web writer for Analytical Methods. She is currently a PhD student at the University of East Anglia, UK.

Detection of nitrite, iodate and bromate

Detection of nitrite, iodate and bromate with Eu-POM sensor

Nitrite, iodate and bromate are commonly found in food and drinking water and they can play important roles in human health. Iodine compounds, for example, are crucial to the smooth running of the thyroid, while bromate is a by-product of water purification. However, the consumption of excessive amounts of these ions can cause serious health issues. Current methods of detecting nitrite, iodate and bromate largely rely on expensive spectroscopic equipment and time consuming chemical analysis.

Li-Hua Bi and Li-Xin Wu from Jilin University, China, have developed a novel detection method which utilises the electrochemistry and redox properties of a europium polyoxometalate (Eu-POM) sensor. The Eu-POM is electrochemically reduced, leading to luminescence quenching and a change in the solution from colourless to blue. The presence of oxidising nitrite, iodate and bromate ions reverses this process, affording discolouration and luminescence recovery. The colour change can be recycled infinitely, and measured using a UV-vis spectrometer. This sensor demonstrates a good linearity relationship between absorbance and concentration of NO2, IO3 and BrO3.

The simplicity of this method, along with high sensitivity and low detection limits, make it an attractive prospect for future use in the sensing of these ions in solution.

A novel detection of nitrite, iodate and bromate based on a luminescent polyoxometalate
Bin Wang,  Rui-Qi Meng,  Ling-Xiao Xu,  Li-Xin Wu and Li-Hua Bi
Anal. Methods, 2013, Advance Article
DOI: 10.1039/C2AY26217G

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More Hot Articles in Issue 2

As well as the wonderful themed papers on Cosmetic Ingredients, we also have a number of brilliant non-themed articles in this latest issue. Topics covered include water analysis, hydrogen peroxide sensing, and CN testing in cells.

A simple and sensitive intramolecular charge transfer fluorescent probe to detect CN− in aqueous media and living cellsA simple and sensitive intramolecular charge transfer fluorescent probe to detect CN in aqueous media and living cells
Mohammad Shahid and Arvind Misra
Anal. Methods, 2013, 5,
DOI: 10.1039/C2AY25921D

Release of iodine from organic matter in natural water by K2S2O8 oxidation for 129I determination
Haijun Dang, Xiaolin Hou, Per Roos and Sven P. Nielsen
Anal. Methods, 2013, 5,
DOI: 10.1039/C2AY25958C

Aqueous synthesis of Ag+ doped CdS quantum dots and its application in H2O2 sensingAqueous synthesis of Ag+ doped CdS quantum dots and its application in H2O2 sensing
Lin Lin, Yaqiong Wen, Yanxia Liang, Na Zhang and Dan Xiao
Anal. Methods, 2013, 5,
DOI: 10.1039/C2AY26063H

These papers will be free to read until January 18th.

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Detecting GHB in Spiked Drinks

Polly-Anna Ashford is a guest web writer for Analytical Methods. She is currently a PhD student at the University of East Anglia, UK.

Detection of GHB in wine

γ-Hydroxybutyrate (GHB) is an odourless, tasteless compound sold illegally as a recreational drug under various names including ‘liquid ecstasy’. However it is more widely known as a date rape drug, causing catalepsy and short term memory loss when added to drinks.  Renato Zenobi and researchers at ETH Zürich report a new application of secondary electrospray ionisation (SESI) mass spectrometry for the detection of GHB in drinks and bodily fluids. The results were found to be consistent across different mass spectrometers and matrices. Both rapid and reliable, this method has the potential to prevent crimes by detecting drugs like GHB (and the structurally related compound GBL) in the headspace of a drink before it is consumed.

This article will be free to read until January 9th. Take a look now:

In situ detection of γ-hydroxybutyrate and γ-butyrolactone in drinks by secondary electrospray ionization
Christian Berchtold, Stefan Schmid, Lukas Meier and Renato Zenobi
Anal. Methods, 2013, Advance Article
DOI: 10.1039/C2AY26009C

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Analytical Methods Issue 2: Cosmetic Ingredients

Cosmetic ingredients: from the cosmetic to the human body and the environment

Chisvert & Salvador, Anal. Methods, 2013, 5,

The second issue of Analytical Methods is online now, and it features papers from a themed issue on Cosmetic Ingredients: from the cosmetic to the human body and the environment. Read all about this topic in the Editorial from Guest Editors Alberto Chisvert and Amparo Salvador from the University of Valencia, Spain. The outside front cover comes from our guest editors and represents the themes from this issue.

Cosmetic ingredients: from the cosmetic to the human body and the environment
Alberto Chisvert and Amparo Salvador
Anal. Methods, 2013, 5, 309-310
DOI: 10.1039/C2AY90060B

Extractive electrospray ionization mass spectrometry for direct characterization of cosmetic products

Chen et al., Anal. Methods, 2013, 5,

On the inside front cover we have an image from Huanwen Chen at East China Institute of Technology, and colleagues from China. In their minireview they have covered the technical developments and applications of extractive electrospray ionization mass spectrometry for the rapid analysis of cosmetic products.

Extractive electrospray ionization mass spectrometry for direct characterization of cosmetic products
Xinglei Zhang, Nannan Wang, Yafei Zhou, Yan Liu, Jinghua Zhang and Huanwen Chen
Anal. Methods, 2013, 5, 311-315
DOI: 10.1039/C2AY25876E

The cover articles will be free to read for 6 weeks.

There are also a number of interesting review papers and exciting research articles on a variety of issues including: analysis of perfumes, surfactants and UV filters in the environment, and microbial contamination of cosmetics. Take a look at a selection of these papers below, they will be free until January 18th.

Fragrances: from essential oils to the human body and atmospheric aerosols
Lai-Hao Wang
Anal. Methods, 2013, 5, 316-322
DOI: 10.1039/C2AY25980J

Current trends in liquid–liquid and solid–liquid extraction for cosmetic analysis: a review
N. Cabaleiro, I. de la Calle, C. Bendicho and I. Lavilla
Anal. Methods, 2013, 5, 323-340
DOI: 10.1039/C2AY25830G

Analytical methods for the characterization and determination of nonionic surfactants in cosmetics and environmental matrices
M. Beneito-Cambra, J. M. Herrero-Martínez and G. Ramis-Ramos
Anal. Methods, 2013, 5, 341-354
DOI: 10.1039/C2AY25847A

A novel outlook on detecting microbial contamination in cosmetic products: analysis of biomarker volatile compounds by solid-phase microextraction gas chromatography-mass spectrometry

A novel outlook on detecting microbial contamination in cosmetic products: analysis of biomarker volatile compounds by solid-phase microextraction gas chromatography-mass spectrometry

Liquid chromatography-tandem mass spectrometry for the multi-residue analysis of organic UV filters and their transformation products in the aquatic environment
Pablo Gago-Ferrero, M. Silvia Díaz-Cruz and Damià Barceló
Anal. Methods, 2013, 5, 355-366
DOI: 10.1039/C2AY26115D

A solid-phase extraction liquid chromatography-tandem mass spectrometry method for the percutaneous absorption assessment of 3-(4′-methylbenzylidene)camphor via human urine analysis
Zacarías León-González, Alberto Chisvert, Isabel Fernández and Amparo Salvador
Anal. Methods, 2013, 5, 367-375
DOI: 10.1039/C2AY25490E

Measurement of iodide and caffeine content in cellulite reduction cosmetic products sold in the European market
Emilia Marchei, Daniela De Orsi, Carmine Guarino, Stefano Dorato, Roberta Pacifici and Simona Pichini
Anal. Methods, 2013, 5, 376-383
DOI: 10.1039/C2AY25761K

A novel outlook on detecting microbial contamination in cosmetic products: analysis of biomarker volatile compounds by solid-phase microextraction gas chromatography-mass spectrometry
Gerardo Alvarez-Rivera, Trinidad De Miguel, Maria Llompart, Carmen Garcia-Jares, Tomas Gonzalez Villa and Marta Lores
Anal. Methods, 2013, 5, 384-393
DOI: 10.1039/C2AY25833A

Take a look at all the papers from this themed issue on Cosmetic Ingredients here.

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Technique to measure chemotherapy effectiveness

A technique to measure how effective chemotherapy is by studying the physical changes that occur in human cells has been developed by US scientists. The method combines atomic force microscopy and Raman spectroscopy to detect biomechanical and biochemical changes in the cells.

The effectiveness of chemotherapy is usually determined by measuring levels of cytokines (cell-signalling proteins) and chemokines (proteins secreted by cells), as well as cell viability, but these traditional methods cannot provide data on single cells, nor do they have the ability to image cells in vitro.

Atomic force microscopy images of (a) cancerous human lung cells and (b) benign human lung cells

To read the full article please visit Chemistry World.

Non-invasive detection of biomechanical and biochemical responses of human lung cells to short time chemotherapy exposure using AFM and Confocal Raman Spectroscopy
Lifu Xiao ,  Mingjie Tang ,  Qifei Li and Anhong Zhou
Anal. Methods, 2012, Accepted Manuscript
DOI: 10.1039/C2AY25951F

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Making criminals leave chemical fingerprints

Scientists in Brazil have shown that luminescent lanthanide tags can be added to ammunition to enable visual identification of gunshot residue at crime scenes, and even on a shooter’s hands, using an ultraviolet lamp.

Scanning electron microscopy-energy dispersive spectroscopy analysis is currently used to identify some types of gunshot residue, but environmental and occupational contamination can give false negatives. The method is also time-consuming and limited by the need to obtain adequate sample quantities. Another problem is that lead-free ammunition is now coming into use to avoid lead pollution and its resulting impact on human health. (The blood level of lead in shooting instructors, for example, is near the limit set out by the National Institute for Occupational Safety and Health of 60µg lead per 100g blood.) But, this ammunition cannot be unequivocally identified, as the techniques used rely on identifying lead as a characteristic compound in gunshot residue.

Luminescent lanthanide-doped ZnAl2O4 added to lead-free ammunition to provide a way to identify lead-free gunshot residue (GSR)

 To read the full article please vist Chemistry World.

ZnAl2O4-based luminescent marker for gunshot residue identification and ammunition traceability
M. A. Melo Lucena ,  G. F. de Sá ,  M. O. Rodrigues ,  S. Alves ,  M. Talhavini and I. T. Weber
Anal. Methods, 2013, Advance Article
DOI: 10.1039/C2AY25535A

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