Miniaturized, high-throughput and green determination of the saponification value of edible oils using thermal infrared enthalpimetry

Nora, Flávia Michelon Dalla; Oliveira, Alessandra Stangherlin; Lucas, Bruna Nichelle; Ferreira, Daniele de Freitas; Duarte, Fábio A.; Mello, Renius; Cichoski, Alexandre José; Barin, Juliano Smanioto

doi:10.1039/c8ay00597d

Cited by 6 publications

(4 citation statements)

References 13 publications

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“…Sample preparation process plays an important role in enhancing sensitivity and reducing matrix interference. The most common preparation technique is saponification [8,9], liquid–liquid extraction (LLE) [10], solid-phase extraction (SPE) [11–14] and derivatization [15]. Saponification is commonly the first step before LLE and SPE and is used to remove neutral lipids, especially triglycerides.…”

Section: Introductionmentioning

confidence: 99%

Salting-out assisted liquid–liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples

et al. 2019

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In this study, salting-out assisted liquid–liquid extraction (SALLE) as a simple and efficient extraction technique followed by high-performance liquid chromatography (HPLC) was employed for the determination of vitamin D3 in milk samples. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. Under the optimum conditions, acetonitrile and ammonium sulfate were used as the extraction solvent and salting-out agent, respectively. The vitamin D3 extract was separated using Hypersil ODS (250x i.d 4.6 mm, 5 µm) HPLC column that was coupled with diode array detector. Vitamin D2 was used as internal standard (IS) to offset any variations in chromatographic conditions. The vitamin D3 and the IS were eluted in 18 min. Good linearity ( r 2 > 0.99) was obtained within the range of 25–600 ng g −1 with the limit of detection of 15 ng g −1 and limit of quantification of 25 ng g −1 . The validated method was applied for the determination of vitamin D3 in milk samples. The recoveries for spiked samples were from 94.4 to 113.5%.

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Section: Introductionmentioning

confidence: 99%

Salting-out assisted liquid–liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples

et al. 2019

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“…17,18 Additionally, it can also be used to determine alcohol content from beverages and the saponification value of edible oils. [19][20][21] Considering the applications in literature for TIE, a reduction in the reagent consumption/waste generation, as well as energy expenditure in one or two orders of magnitude, could generally be obtained in comparison with reference methods. However, TIE can become greener if paper microplates are used, reducing the amount of solvents, samples, and reagents required for analysis and the generation of residues for disposal.…”

Section: Introductionmentioning

confidence: 99%

Thermal Infrared Enthalpimetry in Paper Microzone Plates for Green and High Throughput Determination of Wine Acidities

Ferreira¹,

Tischer²,

Cichoski³

et al. 2020

J. Braz. Chem. Soc.

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The use of paper devices in chemical analysis has been increased due to their low cost, high surface area, portability, and biodegradability. A novel use of paper devices is proposed using thermal infrared enthalpimetry (TIE) for a rapid, green, and high throughput determination of wine acidities. The determination of total, fixed, and volatile acidities in red, white, and sparkling wine was carried out, and the results were compared with AOAC titration method. A multichannel pipette was used for reagent addition and an infrared camera for the temperature monitoring. The pipetting and temperature measurement conditions presented direct influence in the deviations among the measurements. The results obtained by TIE presented an agreement between 96 and 104% with the reference method (AOAC 962.12), for all samples. A high sample throughput was achieved reaching 480 samples h-1 for total acidity. A significant reduction in sample volume and reagent consumption was also obtained, with energy consumption up to 60 times lower in relation to the AOAC method. The association of TIE with a paper device provided a rapid, reliable and green method for the determination of acidities of wines.

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“…The solutions were homogenized under magnetic stirring, and the difference in temperature was related to the limiting reagent (the analyte). This proposed method, called thermal infrared enthalpimetry (TIE), has been successfully used for the analysis of food and drugs in a high throughput and also greener way. − In general, polymeric microplates are used, but recently, some improvements were proposed to reduce the volume of solutions as the reaction in paper microzone plates. , However, the proposed setup used for TIE presented some limitations for field analyses (e.g., the need for stirring) and several parameters (e.g., the total volume of solutions, pipette dispensing rate, and stirring speed) should be adjusted to reach suitable measurements …”

Section: Introductionmentioning

confidence: 99%

Combining In-Tip Reaction and Infrared Thermal Imaging for Fast and Portable Enthalpimetric Analysis

et al. 2020

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In this work, the in-tip thermal infrared enthalpimetry (in-tip TIE) method is proposed for fast enthalpimetric analysis. In this method, the reactions inside the tips of a multichannel pipette were combined with temperature monitoring by an infrared camera. The filter paper was used inside the tips to retain reagents as solutions (wetted paper mode) or as solids (dried paper mode) to perform neutralization, redox, or precipitation reactions. The dried reagents inside the tips were obtained by oven drying a solution retained in the filter paper. The determination of the total acidity of the vinegar, ascorbic acid in vitamin C tablets, and chloride in soy sauces and saline inhalation solutions was performed as examples of the application of the proposed method. The agreement with reference methods ranged from 98 to 107%. The use of reagents dried inside the tip was feasible, leading to a simple aspiration of sample solution within the 12 tips of the pipette to perform a rapid analysis (1 min). Therefore, up to 720 measurements in 1 h were feasible for in-tip TIE over up to 12 measurements for the reference methods. Moreover, miniaturization reduced reagent consumption and residue generation. For example, for in-tip TIE, only 3.6 mL of residues was generated (n = 12) over 60–240 mL in reference methods (n = 3). Contrarily to other TIE methods, no microplates or stirring was required, opening possibilities for field analysis since the multichannel pipette and the infrared camera are both operated with batteries.

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Miniaturized, high-throughput and green determination of the saponification value of edible oils using thermal infrared enthalpimetry

Abstract: Sample preparation and determination steps were performed in microplates using infrared thermography for the residual KOH determination (heat of neutralization).

Cited by 6 publications

References 13 publications

Salting-out assisted liquid–liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples

Salting-out assisted liquid–liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples

Thermal Infrared Enthalpimetry in Paper Microzone Plates for Green and High Throughput Determination of Wine Acidities

Combining In-Tip Reaction and Infrared Thermal Imaging for Fast and Portable Enthalpimetric Analysis

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