The authors would like to acknowledge the support provided to Morgan Philp through an Australian Government Research Training Program Scholarship.

1. Preparation of Color Test Reagent Solutions
NOTE: Weigh 0.12 g of copper nitrate trihydrate into a dry 100 mL beaker. Add 30 mL of deionized (DI) water and carefully swirl it at room temperature to dissolve all solids. Pour this solution into a 100 mL volumetric flask and fill up to the calibrated mark with DI water. This prepared solution is reagent 1. 
NOTE: Reagent 1 can be prepared using other copper(II) salts, e.g. copper(II) chloride.
<ol>
	<li>Weigh 0.11 g of 2,9-dimethyl-1,10-phenanthroline (neocuproine) hemihydrate into a dry 100 mL beaker. Add 50 mL of 0.10 mol/L hydrochloric acid (HCl) and use a glass stirring rod to promote dissolution of solids at room temperature. Pour this solution into a 100 mL volumetric flask and fill up to the calibrated mark with 0.10 mol/L HCl. This prepared solution is reagent 2. 
	CAUTION: Neocuproine is acutely toxic can cause skin irritation and serious eye damage. Wear gloves and safety glasses while handling to minimize the risk of exposure. 
	NOTE: Neocuproine is only slightly soluble in water, therefore, dilute acid is used to prepare this reagent and ensure all solids dissolve.</li>
	<li>Weigh 16.4 g of sodium acetate into a dry 100 mL beaker. Add 50 mL of DI water and use a glass stirring rod to promote dissolution of solids at room temperature. Pour this solution into a 100 mL volumetric flask and fill up to the calibrated mark with DI water. This prepared solution is reagent 3. 
	NOTE: The protocol can be paused here. The reagents are highly stable and can be stored for up to 12 months at room temperature.</li>
</ol>
2. Color Testing
<ol>
	<li>Collect one clean porcelain spot plate, three disposable pipettes, three reagent solutions prepared in step 2.1, one clean spatula, an electric hotplate and the sample/seized material to be tested.</li>
	<li>Using the spatula, place a small, pin-head sized amount (approximately 0.1-0.2 mg) of the unknown sample into three separate wells of a porcelain spot plate. Leave three adjacent wells empty (blank control) and another three wells with equal amounts of 4-methylmethcathinone HCl (4-MMC), a synthetic cathinone reference sample (positive control). 
	NOTE: The preferred test surface is a porcelain spot plate. If these are not available, use plastic microwell plates or semi micro test tubes.</li>
	<li>Using a disposable pipette, add 5 drops of the copper nitrate solution (Reagent 1) to each sample well, in addition to the blank and positive control wells.</li>
	<li>Using a second disposable pipette, add 2 drops of the neocuproine solution (Reagent 2) to each sample well, in addition to the blank and positive control wells.</li>
	<li>Using a third disposable pipette, add 2 drops of the sodium acetate solution (Reagent 3) to each sample well, in addition to the blank and positive control wells. 
	NOTE: The solution turns light blue.</li>
	<li>Place the porcelain spot plate directly onto an electric hotplate set at 80 &#176;C. 
	NOTE: Do not heat plastic microwell plates directly on the hotplate. Prepare a shallow boiling water bath to set the plastic plate. Heat semi-micro test tubes in a small boiling water bath. The precise time required to observe a color change will depend on the thickness and composition of the spot plate. 
	CAUTION: Take care when handling spot plates to prevent burn injuries.</li>
	<li>After heating for 10 min, observe by naked eye and note the final color change or take a photo of the final color change. 
	NOTE: Use a white background to better visualize the color changes.</li>
</ol>

<ol>
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Int. 267, 25-34 (2016).</li><li>United Nations Office on Drugs and Crime (UNODC). <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> World Drug Report 2017. , (2017).</li><li>Australian Criminal Intelligence Commission (ACIC). <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Illicit Drug Data Report 2014-2015. , (2016).</li><li>United Nations Office on Drugs and Crime (UNODC). <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> World Drug Report 2016. , (2016).</li><li>Chatwin, C., Measham, F., O'Brien, K., Sumnall, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=New+drugs,+new+directions?+Research+priorities+for+new+psychoactive+substances+and+human+enhancement+drugs.">New drugs, new directions? Research priorities for new psychoactive substances and human enhancement drugs.</a> Int. J. Drug Policy. 40, 1-5 (2017).</li><li>Reuter, P., Pardo, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=New+psychoactive+substances:+Are+there+any+good+options+for+regulating+new+psychoactive+substances?.">New psychoactive substances: Are there any good options for regulating new psychoactive substances?.</a> Int. J. Drug Policy. 40, 117-122 (2017).</li><li>Elie, M. P., Elie, L. E., Baron, M. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Keeping+pace+with+NPS+releases:+fast+GC-MS+screening+of+legal+high+products.">Keeping pace with NPS releases: fast GC-MS screening of legal high products.</a> Drug Test. 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D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+analysis+in+real+time+mass+spectrometry+(DART-MS)+of+&amp;#34;bath+salt&amp;#34;+cathinone+drug+mixtures.">Direct analysis in real time mass spectrometry (DART-MS) of &amp;#34;bath salt&amp;#34; cathinone drug mixtures.</a> Analyst. 138 (12), 3424-3432 (2013).</li><li>Brown, H., Oktem, B., Windom, A., Doroshenko, V., Evans-Nguyen, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Direct+Analysis+in+Real+Time+(DART)+and+a+portable+mass+spectrometer+for+rapid+identification+of+common+and+designer+drugs+on-site.">Direct Analysis in Real Time (DART) and a portable mass spectrometer for rapid identification of common and designer drugs on-site.</a> Forensic Chem. (Supplement C), 66-73 (2016).</li><li>Bruno, A. M., Cleary, S. R., O'Leary, A. E., Gizzi, M. C., Mulligan, C. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Balancing+the+utility+and+legality+of+implementing+portable+mass+spectrometers+coupled+with+ambient+ionization+in+routine+law+enforcement+activities.">Balancing the utility and legality of implementing portable mass spectrometers coupled with ambient ionization in routine law enforcement activities.</a> Anal Methods-UK. 9 (34), 5015-5022 (2017).</li><li>United Nations Office on Drugs and Crime (UNODC). <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Recommended methods for the identification and analysis of amphetamine, methamphetamine and their ring-substituted analogues in seized materials. , (2006).</li><li>Scientific Working Group for the Analysis of Seized Drugs (SWGDRUG). <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Vol. 7.1. , (2016).</li><li>United Nations Office on Drugs and Crime (UNODC). <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Recommended methods for the identification and analysis of synthetic cathinones in seized materials. , (2015).</li><li>Philp, M., Shimmon, R., Tahtouh, M., Fu, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+and+validation+of+a+presumptive+color+spot+test+method+for+the+detection+of+synthetic+cathinones+in+seized+illicit+materials.">Development and validation of a presumptive color spot test method for the detection of synthetic cathinones in seized illicit materials.</a> Forensic Chem. 1, 39-50 (2016).</li><li>Al-Obaid, A. M., Al-Tamrah, S. A., Aly, F. A., Alwarthan, A. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determination+of+(S)(&#8722;)-cathinone+by+spectrophotometric+detection.">Determination of (S)(&#8722;)-cathinone by spectrophotometric detection.</a> J Pharmaceut Biomed. 17 (2), 321-326 (1998).</li><li>Namera, A., Kawamura, M., Nakamoto, A., Saito, T., Nagao, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Comprehensive+review+of+the+detection+methods+for+synthetic+cannabinoids+and+cathinones.">Comprehensive review of the detection methods for synthetic cannabinoids and cathinones.</a> Forensic Toxicol. 33 (2), 175-194 (2015).</li><li>Isaacs, R. C. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+structure-reactivity+relationship+driven+approach+to+the+identification+of+a+color+test+protocol+for+the+presumptive+indication+of+synthetic+cannabimimetic+drugs+of+abuse.">A structure-reactivity relationship driven approach to the identification of a color test protocol for the presumptive indication of synthetic cannabimimetic drugs of abuse.</a> Forensic Sci. Int. 242, 135-141 (2014).</li></ol>

The authors have nothing to disclose.

This color test protocol was adapted from experimental work published by Al-Obaid et al.18 in which the authors demonstrated a color change occurs in the presence of cathinone extracted from the khat plant. Modifications to the published protocol were necessary to foresee its application in presumptive illicit drug detection. The most important consideration was to reduce the scale of the reaction. The protocol described in the present paper is designed to be applied to street samples and drug seizures.
The described protocol offers a simple presumptive indication of the presence of synthetic cathinones in a sample. Critically, the heating step of the protocol is necessary to visualize the color change of required intensity within the specified time limit. The thickness and composition of the porcelain spot plates may affect the time required for a color change to occur due to the thermal conductivity of the plate material. The 10 min heating period is designed to allow for these differences. Spot plates should also sit flat onto the hotplate so all wells experience the same amount of heat. Heating the spot plates longer than 10 min or at temperatures above 80 &#176;C can affect the results negatively through the evaporation of the aqueous solutions. A second critical step is the addition of all three reagents, as the protocol will fail to work without all three.
Presumptive color tests are designed to be selective toward a certain drug class; provide results with rapidity, and possess a degree of portability to allow application in the field. The requirement of a heat source significantly decreases the portability of the test method. In addition, the 10 min heating period is not an ideal length of time to wait for a presumptive color test and is a limitation of this test protocol.
The basis of the color change occurring in this protocol is a non-specific reduction-oxidation reaction, which means that the synthetic cathinone molecules are not a ligand in the final colored complex. This inherent non-specific reaction means that there are likely other species that will interfere and reduce the copper(II) ions, e.g. ascorbic acid, and therefore lower the test specificity.
All presumptive color tests for illicit drugs are a subjective form of analysis based on the analyst&#39;s color perception. The color test protocol proposed here is particularly simple due to only one color change indicative of synthetic cathinone presence. This is unlike many general screening color tests that afford several different hues depending on the drug present.
This paper describes a useful and novel protocol for presumptively suggesting the presence of synthetic cathinones in seized material prior to confirmatory analysis. Commonly employed color test reagents are not able to afford the required specificity offered by the copper-neocuproine reagent. The most commonly used general screening color test reagent, Marquis, has been shown to afford negative results for many synthetic cathinones19. Although the Liebermann&#39;s reagent does react with cathinones, it also reacts with other illicit materials, including many synthetic cannabinoids20.
The application of this protocol is ideal for forensic drug testing laboratories employing presumptive testing of seized samples. The reagent solutions are highly stable, and the protocol itself is particularly easy to follow.

The illicit drug market operates similarly to a traditional business by continuing to evolve and adapt to a changing marketplace. Advances in modern technology, specifically, the global proliferation of powerful communication has seen increased online purchases via the Dark Net1 and extensive knowledge sharing among users via online forums2. Combined with advances in chemistry, the rapid emergence of new psychoactive substances (NPS) created a serious challenge for international and national drug control.
NPS are potentially dangerous substances of abuse that have similar effects to drugs under international control. Initially marketed as &#34;legal&#34; alternatives, 739 NPS were reported to the United Nations Office on Drugs and Crime (UNODC) between 2009 and 20163. According to the most recent annual report, a record number of NPS were seized at the Australian border, with the majority of those analyzed, further identified as synthetic cathinones4. On a global scale, seizures of synthetic cathinones have been steadily increasing since first reported in 2010, and are one of the most commonly seized NPS5.
The challenges posed by NPS have been a largely published topic of discussion6,7. Forensic laboratories and law enforcement personnel were left at a disadvantage without appropriate methods in place to detect and identify NPS during their rapid emergence. Extensive research into the detection of NPS, including synthetic cathinones, in seized material, has employed gas chromatography-mass spectrometry (GC-MS)8 and liquid chromatography-high resolution mass spectrometry (LC-HRMS)9 for confirmatory analysis. Increasing demand for minimal sample preparation has seen infrared and Raman spectroscopy10 studies as well as ambient ionisation mass spectrometric analyses, such as direct analysis in real time mass spectrometry (DART-MS)11,12. The need for rapid, sensitive analysis in the field has also seen the incorporation of paper spray ionization-mass spectrometry (PSI-MS) into portable devices for use by law enforcement13. Many instrumental techniques offer confirmatory analysis with sensitive detection and quantitative results. However, for high-throughput analysis, they can be time-consuming due to sample preparation, run times, and instrument training and maintenance.
Presumptive color tests are designed to suggest the presence or absence of certain drug classes in a test sample14. The Scientific Working Group for the Analysis of Seized Drugs (SWGDRUG) classifies color testing as the lowest discriminating power technique, alongside ultraviolet spectroscopy and immunoassays15. However, they are still widely employed by law enforcement and other security personnel as a means to provide rapid results at a significantly lower cost compared to other techniques. The main advantage offered by color spot test methods is the ability to perform them in the field using portable test kits.
The selectivity of color tests relies on individual chemical reactions occurring between the test reagent and the drug class of interest to create a color change. Current presumptive testing protocols lack a particular test for detecting synthetic cathinones only; commonly used reagents that lack specificity and contain hazardous substances are often employed. Other recommended reagents have not been screened on a large number of possible synthetic cathinone substances16.
The aim of this work is to present a simple color test protocol that can be easily employed by interested parties for the preliminary screening of synthetic cathinones in illicit substances of unknown composition. Interested parties would include law enforcement, border protection agencies, forensic laboratories, and other relevant security personnel. The proposed methods employ a reduction-oxidation reaction occurring between the electron-accepting copper complex reagent and the electron rich synthetic cathinone drug molecules. Using these chemical methods developed, one can apply them in the form of a presumptive color test to suggest the presence of synthetic cathinones.

color spot test as a presumptive tool for the rapid detection of synthetic cathinones

Synthetic cathinones are a large class of new psychoactive substances (NPS) that are increasingly prevalent in drug seizures made by law enforcement and other border protection agencies globally. Color testing is a presumptive identification technique indicating the presence or absence of a particular drug class using rapid and uncomplicated chemical methods. Owing to their relatively recent emergence, a color test for the specific identification of synthetic cathinones is not currently available. In this study, we introduce a protocol for the presumptive identification of synthetic cathinones, employing three aqueous reagent solutions: copper(II) nitrate, 2,9-dimethyl-1,10-phenanthroline (neocuproine) and sodium acetate. Small pin-head sized amounts (approximately 0.1-0.2 mg) of the suspected drugs are added to the wells of a porcelain spot plate, and each reagent is then added dropwise sequentially before heating on a hotplate. A color change from very light blue to yellow-orange after 10 min indicates the likely presence of synthetic cathinones. The highly stable and specific test reagent has the potential for use in the presumptive screening of unknown samples for synthetic cathinones in a forensic laboratory. However, the nuisance of an added heating step for the color change result limits the test to laboratory application and decreases the likelihood of an easy translation to field testing.

The test protocol has been validated through several studies, the results of which are described in Philp et al.17. The color test method is able to presumptively detect synthetic cathinones in an unknown sample through a color change from light blue to yellow-orange (Figure 1). Yellow and orange color changes occuring after the heating period are considered positive test results and any other color change, including very weak yellow or changes occurring before heatingare considered negative (Table 1).
The protocol has been applied to 44 synthetic cathinone analogues, 44 other illicit drugs, and 36 miscellaneous powders and cutting agents in previously published work17. Color changes experienced by these substances is summarized in the Supplementary File 1. These studies illustrate the success of the protocol in presumptively identifying the presence of synthetic cathinones. The test protocol showed an 89% true positive test rate and a false positive rate of 10%. Representative positive test results are illustrated in Figure 2, and representative negative test results are provided in Figure 3. This test protocol can also successfully identify the presence of synthetic cathinones in mixtures containing more than one compound (Figure 4). This is an important result demonstrating its applicability to real-world samples.
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/57045/57045fig1.jpg" /> 
Figure 1: Representative results from the color test protocol performed on a porcelain spot plate. (A) Color remains light blue with reagents only (blank control). (B) Yellow-orange color change with synthetic cathinone, 4-methylmethcathinone HCl (positive control). <a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57045/57045fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/57045/57045fig2.jpg" /> 
Figure 2: Representative positive results from the color test protocol performed on a porcelain spot plate. The range of colors seen in a positive result is due to differences in antioxidant capacity and solubility of the compounds. (A) Yellow-orange color change with synthetic cathinone, N,N-dimethylcathinone HCl (true positive). (B) Light yellow-orange color change with synthetic cathinone, 3,4-dimethylmethcathinone HCl (true positive). (C) Light orange color change with a green ring around the edge with synthetic cathinone, 2,4,5-trimethylmethcathinone HCl (true positive). (D) Yellow color change with piperazine analog, 1-[3-(trifluoromethyl)phenyl]piperazine (TFMPP) HCl (false positive). <a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57045/57045fig2large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Figure 3" class="xfigimg" src="/files/ftp_upload/57045/57045fig3.jpg" /> 
Figure 3: Representative negative results from the color test protocol performed on a porcelain spot plate. (A) Light green color change with synthetic cathinone, 3,4-methylenedioxy-&#945;-pyrrolidinobutiophenone (MDPBP) HCl (false negative). (B) Blue color change with miscellaneous powder, glycine (true negative). (C) Orange color change with drug precursor, 3,4-methylenedioxyphenyl-2-propanone (MDP2P) occurred before heating (true negative). (D) Color remained light blue with amphetamine sulfate (true negative). <a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57045/57045fig3large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Figure 4" class="xfigimg" src="/files/ftp_upload/57045/57045fig4.jpg" /> 
Figure 4: Representative results of performing the color test protocol on mixtures of compounds. (A) Yellow-orange color change with a mixture of 4-methylmethcathinone HCl and ephedrine HCl. (B) A yellow-orange color change with a mixture of 4-methylmethcathinone HCl and 4-fluoromethcathinone (4-FMC) HCl. <a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57045/57045fig4large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Table" class="xfigimg" src="/files/ftp_upload/57045/57045table1.jpg" /> 
Table 1: Color changes observed using the color test protocol. The proposed copper-neocuproine color test protocol was applied to 124 different substances and the color changes were recorded. Yellow and orange colors indicate a positive test result, while any other color is reported as a negative result.
Supplementary File 1. Color test results for substrates. <a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/57045/Supplementary_material.xlsx">Please click here to download this file.</a>

Watch this Scientific Journal Video about Color Spot Test As a Presumptive Tool for the Rapid Detection of Synthetic Cathinones at JoVE.com

Color Spot Test As a Presumptive Tool for the Rapid Detection of Synthetic Cathinones

Here we present a simple, inexpensive, and selective chemical spot test protocol for the detection of synthetic cathinones, a class of new psychoactive substances. The protocol is suitable for use in various areas of law enforcement that encounter illicit material.

Synthetic cathinones are a large class of new psychoactive substances (NPS) that are increasingly prevalent in drug seizures made by law enforcement and ...

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Nanyang Technological University

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24.5K Views.  University of Technology Sydney (UTS). Here we present a simple, inexpensive, and selective chemical spot test protocol for the detection of synthetic cathinones, a class of new psychoactive substances. The protocol is suitable for use in various areas of law enforcement that encounter illicit material.

Video: Color Spot Test As a Presumptive Tool for the Rapid Detection of Synthetic Cathinones

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We demonstrate a method to fabricate highly sensitive surface-enhanced Raman spectroscopic (SERS) substrates using a filter syringe system that can be ...

HKUST-1 as a Heterogeneous Catalyst for the Synthesis of Vanillin

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately 200 different odorant compounds in addition to vanillin. The natural extraction of vanillin (from the orchid Vanilla planifolia, Vanilla tahitiensis and Vanilla pompon) represents only 1% of the worldwide production and since this process is expensive and very long, the rest of the production of vanillin is synthesized. Many biotechnological approaches can be used for the synthesis of vanillin from lignin, phenolic stilbenes, isoeugenol, eugenol, guaicol, etc., with the disadvantage of harming the environment since these processes use strong oxidizing agents and toxic solvents. Thus, eco-friendly alternatives on the production of vanillin are very desirable and thus, under current investigation. Porous coordination polymers (PCPs) are a new class of highly crystalline materials that recently have been used for catalysis. HKUST-1 (Cu3(BTC)2(H2O)3, BTC = 1,3,5-benzene-tricarboxylate) is a very well known PCP which has been extensively studied as a heterogeneous catalyst. Here, we report a synthetic strategy for the production of vanillin by the oxidation of trans-ferulic acid using HKUST-1 as a catalyst.

The conversion of trans-ferulic acid to vanillin was achieved by heterogeneous catalysis. HKUST-1 was employed in this synthesis and the essential step in the catalytic process was the generation of unsaturated metal sites. Thus, when the catalyst was activated under vacuum, full vanillin conversion (yield of 95%) was obtained.

Vanillin (4-hydoxy-3-methoxybenzaldehyde) is the main component of the extract of vanilla bean. The natural vanilla scent is a mixture of approximately ...

Using Capillary Electrophoresis to Quantify Organic Acids from Plant Tissue: A Test Case Examining Coffea arabica Seeds

Carboxylic acids are organic acids containing one or more terminal carboxyl (COOH) functional groups. Short chain carboxylic acids (SCCAs; carboxylic acids containing three to six carbons), such as malate and citrate, are critical to the proper functioning of many biological systems, where they function in cellular respiration and can serve as indicators of cell health. In foods, organic acid content can have significant impact on taste, with increased SCCA levels resulting in a sour or &#34;acid&#34; taste. Because of this, methods for the rapid analysis of organic acid levels are of particular interest to the food and beverage industries. Unfortunately, however, most methods used for SCCA quantification are dependent on time-consuming protocols requiring the derivatization of samples with hazardous reagents, followed by costly chromatographic and/or mass spectrometric analyses. This method details an alternate method for the detection and quantification of organic acids from plant material and food samples using free zonal capillary electrophoresis (CZE), sometimes simply referred to as capillary electrophoresis (CE). CZE provides a cost-effective method for measuring SCCAs with a low limit of detection (0.005 mg/ml). This article details the extraction and quantification of SCCAs from plant samples. While the method provided focuses on measurement of SCCAs from coffee beans, the method provided can be applied to multiple plant-based food materials.

Using Capillary Electrophoresis to Quantify Organic Acids from Plant Tissue: A Test Case Examining Coffea arabica Seeds

This article presents a method for the detection and quantification of organic acids from plant material using free zonal capillary electrophoresis. An example of the potential application of this method, determining the effects of a secondary fermentation on organic acid levels in coffee seeds, is provided.

Carboxylic acids are organic acids containing one or more terminal carboxyl (COOH) functional groups. Short chain carboxylic acids (SCCAs; carboxylic ...

NMR Spectroscopy as a Robust Tool for the Rapid Evaluation of the Lipid Profile of Fish Oil Supplements

The western diet is poor in n-3 fatty acids, therefore the consumption of fish oil supplements is recommended to increase the intake of these essential nutrients. The objective of this work is to demonstrate the qualitative and quantitative analysis of encapsulated fish oil supplements using high-resolution 1H and 13C NMR spectroscopy utilizing two different NMR instruments; a 500 MHz and an 850 MHz instrument. Both proton (1H) and carbon (13C) NMR spectra can be used for the quantitative determination of the major constituents of fish oil supplements. Quantification of the lipids in fish oil supplements is achieved through integration of the appropriate NMR signals in the relevant 1D spectra. Results obtained by 1H and 13C NMR are in good agreement with each other, despite the difference in resolution and sensitivity between the two nuclei and the two instruments. 1H NMR offers a more rapid analysis compared to 13C NMR, as the spectrum can be recorded in less than 1 min, in contrast to 13C NMR analysis, which lasts from 10 min to one hour. The 13C NMR spectrum, however, is much more informative. It can provide quantitative data for a greater number of individual fatty acids and can be used for determining the positional distribution of fatty acids on the glycerol backbone. Both nuclei can provide quantitative information in just one experiment without the need of purification or separation steps. The strength of the magnetic field mostly affects the 1H NMR spectra due to its lower resolution with respect to 13C NMR, however, even lower cost NMR instruments can be efficiently applied as a standard method by the food industry and quality control laboratories.

Here, high-resolution 1H and 13C Nuclear Magnetic Resonance (NMR) spectroscopy was used as a rapid and reliable tool for quantitative and qualitative analysis of encapsulated fish oil supplements.

The western diet is poor in n-3 fatty acids, therefore the consumption of fish oil supplements is recommended to increase the intake of these essential ...

Coulomb Explosion Imaging as a Tool to Distinguish Between Stereoisomers

This article shows how the COLTRIMS (Cold Target Recoil Ion Momentum Spectroscopy) or the "reaction microscope" technique can be used to distinguish between enantiomers (stereoisomers) of simple chiral species on the level of individual molecules. In this approach, a gaseous molecular jet of the sample expands into a vacuum chamber and intersects with femtosecond (fs) laser pulses. The high intensity of the pulses leads to fast multiple ionization, igniting a so-called Coulomb Explosion that produces several cationic (positively charged) fragments. An electrostatic field guides these cations onto time- and position-sensitive detectors. Similar to a time-of-flight mass spectrometer, the arrival time of each ion yields information on its mass. As a surplus, the electrostatic field is adjusted in a way that the emission direction and the kinetic energy after fragmentation lead to variations in the time-of-flight and in the impact position on the detector.
Each ion impact creates an electronic signal in the detector; this signal is treated by high-frequency electronics and recorded event by event by a computer. The registered data correspond to the impact times and positions. With these data, the energy and the emission direction of each fragment can be calculated. These values are related to structural properties of the molecule under investigation, i.e. to the bond lengths and relative positions of the atoms, allowing to determine molecule by molecule the handedness of simple chiral species and other isomeric features.

For small chiral species, Coulomb Explosion Imaging provides a new approach to determine the handedness of individual molecules.

This article shows how the COLTRIMS (Cold Target Recoil Ion Momentum Spectroscopy) or the "reaction microscope" technique can be used to distinguish ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

A Facile Synthetic Method to Obtain Bismuth Oxyiodide Microspheres Highly Functional for the Photocatalytic Processes of Water Depuration

Bismuth oxyhalide (BiOI) is a promising material for sunlight-driven-environmental photocatalysis. Given that the physical structure of this kind of materials is highly related to its photocatalytic performance, it is necessary to standardize the synthetic methods in order to obtain the most functional architectures and, thus, the highest photocatalytic efficiency. Here, we report a reliable route to obtain BiOI microspheres via the solvothermal process, using Bi(NO3)3 and potassium iodide (KI) as precursors, and ethylene glycol as a template. The synthesis is standardized in a 150 mL autoclave, at 126 &#176;C for 18 h. This results in 2-3 &#181;m-sized mesoporous microspheres, with a relevant specific surface area (61.3 m2/g). Shortening the reaction times in the synthesis results in amorphous structures, while higher temperatures lead to a slight increase in the porosity of the microspheres, with no effect in the photocatalytic performance. The materials are photo-active under UV-A/visible light irradiation for the degradation of the antibiotic ciprofloxacin in water. This method has demonstrated to be effective in interlaboratory tests, obtaining similar BiOI microspheres in Mexican and Chilean research groups.

This article describes a synthetic method to obtain bismuth oxyiodide microspheres, which are highly functional to perform the photocatalytic removal of organic pollutants, such as ciprofloxacin, in water under UV-A/visible light irradiation.

Bismuth oxyhalide (BiOI) is a promising material for sunlight-driven-environmental photocatalysis. Given that the physical structure of this kind of ...

An Electrochemical Cholesteric Liquid Crystalline Device for Quick and Low-Voltage Color Modulation

We demonstrate a method for fabricating a prototype reflective display device that contains cholesteric liquid crystal (LC) as an active component. The cholesteric LC is composed of a nematic LC 4&#39;-pentyloxy-4-cyanobiphenyl (5OCB), redox-responsive chiral dopant (FcD), and a supporting electrolyte 1-ethyl-3-methylimidazolium trifluoromethanesulfonate (EMIm-OTf). The most important component is FcD. This molecule changes its helical twisting power (HTP) value in response to redox reactions. Therefore, in situ electrochemical redox reactions in the LC mixture allow for the device to change its reflection color in response to electrical stimuli. The LC mixture was introduced, by a capillary action, into a sandwich-type ITO glass cell comprising two glass slides with patterned indium tin oxide (ITO) electrodes, one of which was coated with poly(3,4-ethylenedioxythiophene)-co-poly(ethylene glycol) doped with perchlorate (PEDOT+). Upon application of +1.5 V, the reflection color of the device changed from blue (467 nm) to green (485 nm) in 0.4 s. Subsequent application of 0 V made the device recover the original blue color in 2.7 s. This device is characterized by its fastest electrical response and lowest operating voltage among any previously reported cholesteric LC device. This device could pave the way for the development of next generation reflective displays with low energy consumption rates.

A protocol for the fabrication of a reflective cholesteric liquid crystalline display device containing a redox-responsive chiral dopant allowing quick and low-voltage operation is presented.

We demonstrate a method for fabricating a prototype reflective display device that contains cholesteric liquid crystal (LC) as an active component. The ...

Color Spot Test As a Presumptive Tool for the Rapid Detection of Synthetic Cathinones

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Stabilizing Hepatocellular Phenotype Using Optimized Synthetic Surfaces

Optimization of Synthetic Proteins: Identification of Interpositional Dependencies Indicating Structurally and/or Functionally Linked Residues

A Filter-based Surface Enhanced Raman Spectroscopic Assay for Rapid Detection of Chemical Contaminants

HKUST-1 as a Heterogeneous Catalyst for the Synthesis of Vanillin

Using Capillary Electrophoresis to Quantify Organic Acids from Plant Tissue: A Test Case Examining Coffea arabica Seeds

NMR Spectroscopy as a Robust Tool for the Rapid Evaluation of the Lipid Profile of Fish Oil Supplements

Coulomb Explosion Imaging as a Tool to Distinguish Between Stereoisomers

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

A Facile Synthetic Method to Obtain Bismuth Oxyiodide Microspheres Highly Functional for the Photocatalytic Processes of Water Depuration

An Electrochemical Cholesteric Liquid Crystalline Device for Quick and Low-Voltage Color Modulation