scholarly journals Comparison of Two Extraction Procedures, SPE and DLLME, for Determining Plasticizer Residues in Hot Drinks at Vending Machines

Processes ◽  
2021 ◽  
Vol 9 (9) ◽  
pp. 1588
Author(s):  
Ivan Notardonato ◽  
Sergio Passarella ◽  
Alessia Iannone ◽  
Cristina Di Fiore ◽  
Mario Vincenzo Russo ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Enrichment Factors ◽  
Limit Of Quantification ◽  
Extraction Procedures ◽  
Vending Machines ◽  
The Matrix ◽  
Decaffeinated Coffee ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

This paper would like to compare two extraction procedures for analyzing phthalates (PAEs) in hot drinks collected at vending machines, usually coffee and tea. The two analytical procedures are based on Solid Phase Extraction (SPE) using C18 cartridge and on dispersive liquid-liquid microextraction (DLLME) assisted by ultrasound and vortex for improving the dispersion mechanically, with each followed by a routinary analytical method such as GC-FID. Seven phthalates (DMP, DEP, DiBP, DBP, DEHP, DOP, DDP) have been analyzed and determined. All the analytical parameters (i.e., recovery, limit of detection, limit of quantification, enrichment factors, repeatability, reproducibility) have been investigated and discussed, as has the matrix effect. The entire procedure has been applied to hot drink matrices, e.g., coffee, decaffeinated coffee, barley coffee, ginseng coffee and tea.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

scholarly journals Analytical Scheme for Simultaneous Determination of Phthalates and Bisphenol A in Honey Samples Based on Dispersive Liquid–Liquid Microextraction Followed by GC-IT/MS. Effect of the Thermal Stress on PAE/BP-A Levels

2020 ◽  
Vol 3 (1) ◽  
pp. 23 ◽  
Author(s):  
Ivan Notardonato ◽  
Sergio Passarella ◽  
Giuseppe Ianiri ◽  
Cristina Di Fiore ◽  
Mario Vincenzo Russo ◽  
...  
Keyword(s):  
Bisphenol A ◽  
Simultaneous Determination ◽  
Thermal Stresses ◽  
Ion Trap ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Analytical Scheme ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

In this paper, an analytical protocol was developed for the simultaneous determination of phthalates (di-methyl phthalate DMP, di-ethyl phthalate DEP, di-isobutyl phthalate DiBP, di-n-butyl phthalate DBP, bis-(2-ethylhexyl) phthalate DEHP, di-n-octyl phthalate DNOP) and bisphenol A (BPA). The extraction technique used was the ultrasound vortex assisted dispersive liquid–liquid microextraction (UVA-DLLME). The method involves analyte extraction using 75 µL of benzene and subsequent analysis by gas chromatography combined with ion trap mass spectrometry (GC-IT/MS). The method is sensitive, reliable, and reproducible with a limit of detection (LOD) below 13 ng g−1 and limit of quantification (LOQ) below 22 ng g−1 and the intra- and inter-day errors below 7.2 and 9.3, respectively. The method developed and validated was applied to six honey samples (i.e., four single-use commercial ones and two home-made ones. Some phthalates were found in the samples at concentrations below the specific migration limits (SMLs). Furthermore, the commercial samples were subjected to two different thermal stresses (24 h and 48 h at 40 °C) for evidence of the release of plastic from the containers. An increase in the phthalate concentrations was observed, especially during the first phase of the shock, but the levels were still within the limits of the regulations.

scholarly journals Determination of Budesonide and Sulfasalazine in Water and Wastewater Samples Using DLLME-SFO-HPLC-UV Method

Water ◽  
2019 ◽  
Vol 11 (8) ◽  
pp. 1581 ◽  
Author(s):  
Hryniewicka ◽  
Starczewska ◽  
Gołębiewska
Keyword(s):  
Ionic Strength ◽  
Limit Of Detection ◽  
Enrichment Factors ◽  
Aqueous Samples ◽  
Calibration Curves ◽  
Water And Wastewater ◽  
Wastewater Samples ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

Dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) was applied to isolate budesonide (BUD) and sulfasalazine (SULF) from aqueous samples. The effects of different parameters on the efficiency on the extraction such as type of extrahent and dispersive solvent, ionic strength, pH of sample, and centrifugation time were investigated. Moreover, the influence of foreign substances on a studied process was tested. The calibration curves were recorded. The linearity ranges for BUD and SULF were 0.022–8.611 µg mL−1 and 0.020–7.968 µg mL−1 with the limit of detection (LOD) 0.011 µg mL−1 and 0.012 µg mL−1, respectively. The enrichment factors (EF) for two analytes were high: for BUD it was 145.7 and for SULF, 119.5. The elaborated procedure was applied for HPLC-UV determination of these analytes in water and wastewater samples.

scholarly journals Establishment and Validation of a GC–MS/MS Method for the Quantification of Penicillin G Residues in Poultry Eggs

Foods ◽  
2021 ◽  
Vol 10 (11) ◽  
pp. 2735
Author(s):  
Chujun Liu ◽  
Yawen Guo ◽  
Bo Wang ◽  
Lan Chen ◽  
Kaizhou Xie ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Egg Yolk ◽  
Calibration Method ◽  
Penicillin G ◽  
Limit Of Quantification ◽  
Poultry Eggs ◽  
Relative Standard ◽  
The Matrix ◽  
Trimethylsilyl Diazomethane

A simple and sensitive gas chromatography–tandem mass spectrometry (GC–MS/MS) method was established for the quantitative screening of penicillin G residues in chicken and duck eggs (whole egg, yolk and albumen). The analyte was separated on a TG-1MS capillary column (30.0 m × 0.25 mm i.d., 0.25 μm) with an external calibration method and electron impact (EI) ionization. Samples were pretreated using an accelerated solvent extraction (ASE) procedure followed by solid-phase extraction (SPE) on HLB cartridges (60 mg/3 mL). The derivative, which was safer and easier to store than penicillin G, was obtained by reacting trimethylsilyl diazomethane (TMSD) with penicillin G. The method was validated by the following parameters: linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ). The matrix-matched calibration curves had good linearity (R2 ≥ 0.9994) within the concentration range of LOQ–200.0 µg/kg for penicillin G in the sample matrices. In the same concentration range, the accuracy, in terms of recovery, was 80.31–94.50%; the relative standard deviation (RSD), intra-day RSD and inter-day RSD ranged from 1.24 to 3.44%, 2.13 to 4.82% and 2.74 to 6.13%, respectively. The LODs and LOQs of penicillin G in the matrices were in the ranges of 1.70–3.20 and 6.10–8.50 μg/kg, respectively. The applicability of the GC–MS/MS method was demonstrated by the determination of poultry eggs obtained from local markets with no penicillin G residues.

scholarly journals Dispersive Liquid-Liquid Microextraction in the Analysis of Milk and Dairy Products: A Review

2016 ◽  
Vol 2016 ◽  
pp. 1-12 ◽  
Author(s):  
Andrew Quigley ◽  
Wayne Cummins ◽  
Damian Connolly
Keyword(s):  
Dairy Products ◽  
Solid Phase ◽  
Sample Pretreatment ◽  
Enrichment Factors ◽  
Extraction Methods ◽  
Aqueous Sample ◽  
Preparation Technique ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction ◽  
Very High

Dispersive liquid-liquid microextraction (DLLME) is an extraction technique developed within the last decade, which involves the dispersion of fine droplets of extraction solvent in an aqueous sample. Partitioning of analytes into the extraction phase is instantaneous due to the very high collective surface area of the droplets. This leads to very high enrichment factors and very low solvent consumption, relative to other liquid or solid phase extraction methods. A comprehensive review of the various modes of DLLME in the analysis of organic and inorganic analytes in dairy products (milk, cheese, infant formula, yogurt, and breast milk) is presented here. Dairy products present a complex sample matrix and the removal of interfering matrix components can prove troublesome. This review focuses on sample pretreatment prior to the appropriate DLLME procedure, the extraction and dispersive solvents chosen, derivatisation methods, and analytical figures of merit. Where possible, a critical comparison of DLLME methods has been undertaken. The overall suitability, and limitations, of DLLME as a sample preparation technique for dairy products has been assessed.

scholarly journals Spectrophotometric Determination of Zirconium by Dispersive Liquid-Liquid Microextraction based on Solidification of Floating Organic Droplets

2020 ◽  
Vol 32 (12) ◽  
pp. 3191-3196
Author(s):  
Intizam Ahmadov
Keyword(s):  
Spectrophotometric Determination ◽  
Limit Of Detection ◽  
Ph Effect ◽  
Ionic Surfactant ◽  
Ligand Effect ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

In this study, a new method was developed for the spectrophotometric determination of zirconium by the procedure of dispersive liquid-liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO). o-Nitrobenzene-azopyrocatechol (o-NBAP) and non-ionic surfactant (OP-10) were used in the complex formation. At the first stage, a separation and solidification processes were carried out, after which the solidified samples were examined by spectrophotometric method. The effect of various parameters viz. pH effect, ion resistance, ligand effect, volume and type of extraction and dispersion solution, extraction time and temperature effect were studied. The results of the experiment were optimized with design programs. The calibration curve was linear ranging from 0.5 to70 μg L-1, with a correlation coefficient of 0.998. The limit of detection (LOD) is 0.12 μg L-1, the limit of quantification (LOQ) is 0.40 μg L-1 and the relative standard deviation (RSD) at 60 μg L-1 is 1.6% (n=6). This method was also applied to determine zirconium in various water samples. The obtained reextraction amount was 98-110%.

Determination of phthalate esters in seawater of Chabahar Bay using dispersive liquid-liquid microextraction coupled with GC-FID

2017 ◽  
Vol 77 (7) ◽  
pp. 1782-1790 ◽  
Author(s):  
Beheshteh Ajdari ◽  
Mahmoud Nassiri ◽  
Mir Mahdi Zahedi ◽  
Morteza Ziyaadini
Keyword(s):  
Sea Water ◽  
Limit Of Detection ◽  
Phthalate Esters ◽  
Environmental Pollutants ◽  
Enrichment Factors ◽  
Chabahar Bay ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

Abstract Phthalate esters (PEs), a group of environmental pollutants which are possibly carcinogenic to humans, have been detected in seawater. Seven PEs in seawater were quantitatively determined by using gas-chromatography flame ionizing detection after executing dispersive liquid-liquid microextraction. The suggested method is optimized for microextraction and determination of PEs in artificial sea water. Factors affecting the microextraction procedure such as the type and volume of extracting and dispersive solvents (carbon tetrachloride, 20 μL; methanol, 0.5 mL), extraction time and pH (7) were investigated. Under optimum conditions, the limit of detection of the analytes were obtained between 0.04 and 4.52 μg·L−1, and linearity and linear range were of 0.999 ≥ R2 ≥ 0.994 and 10–560 μg·L−1 respectively. Enrichment factors were found in the range of 761–827 fold, while the relative standard deviations of the analytes were between 0.17 and 7.5% (n = 6) for real sea water samples. Using this method, total PEs content of seawater from several locations in Chabahar Bay (the southeast part of Iran) was estimated 2.33–90.45 μg·L−1.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

Sign in / Sign up

Export Citation Format

Share Document