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 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.

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%).

Detecting PAEs in Bottled Water by SPE-LC/QQQ

2013 ◽  
Vol 469 ◽  
pp. 444-449
Author(s):  
Yu Zi Liu ◽  
Ying Hao Xing ◽  
Jun Wu
Keyword(s):  
Drinking Water ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Bottled Water ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
The Common ◽  
Acid Esters

In this study, High Performance Liquid Chromatography (HPLC), combined with Triple Quadruple mass Spectrometry (QQQ) were developed and applied in the analysis of 16 phthalic acid esters (PAEs) in the common drinking water. Qualitative and quantitative analysis were carried out by Multiple Reaction Monitoring (MRM). The method, combined with Solid Phase Extraction, was established to detect the PAEs in drinking water. As showed by the results, 16 PAEs had a good linearity in the range of 1.14~101.4μg/L, with correlation coefficient between 0.996~0.999. The mean recoveries were in the range of 87.53~131.37%, with the relative standard deviation be 0.71~5.09%. The limit of quantification (LOQ) of 16 PAEs were between 1.14~32.51μg/L, with the limit of detection (LOD) be 0.34~10.67μg/L. There were five PAEs which were detected in the range of <1.7~17.2μg/L in bottled water. Some products have some PAEs which havent been shown in the national or the international standard of the drinking water.

scholarly journals Preparation of a new coating of graphene oxide/nickel complex on a nickelized metal surface for direct immersion solid phase microextraction of some polycyclic aromatic hydrocarbons

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Yalda Pasandideh ◽  
Habib Razmi
Keyword(s):  
Graphene Oxide ◽  
Solid Phase Microextraction ◽  
High Efficiency ◽  
Mechanical Stability ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Limit Of Quantification ◽  
Coating Materials ◽  
Relative Standard ◽  
Validation Parameters

Abstract Background Solid-phase microextraction (SPME) is a versatile sampling and sample preparation technology that possess a significant application in the extraction and pre-concentration of a broad range of micro-pollutants from different kind of matrices. Selection and preparation of an appropriate fiber substrate and coating materials have always been the main challenges of the SPME procedure. This paper introduces a high-efficiency metal-based SPME fiber with a new chemical coating of nickel/graphene oxide/nickel tetraazamacrocyclic complex (Ni/GO/NiTAM). Result The Ni/GO/NiTAM sorbent was electroless deposited onto the surface of an aluchrom (Alu) wire, and then the prepared fiber was employed for the extraction and pre-concentration of some PAHs before their HPLC–UV analysis. The prepared fiber characterization data were assessed using FE-SEM, EDX, XRD, FT-IR, and BET techniques. The method validation parameters, including the linearity range (LRs: 0.10 to 200.0 µg L−1), the limit of detection (LODs: 0.03‒0.30 µg L−1), and the limit of quantification (LOQs: 0.10–1.00 µg L−1), under optimal conditions. The relative standard deviations (RSDs) of intra-day, inter-day, and single fiber repeatability (for the samples spiked at 25 µg L‒1) were in the range of 0.32–2.94, 1.20–4.09, and 1.42‒4.39%, respectively. In addition, the technique recoveries (RR %) and enrichment factors (EF) were in the range of 83.10‒107.80% and 83–164, respectively. Conclusion The fiber fabrication was simple, and the applied materials were also economical and easily accessible. Alu metal has high physicochemical and mechanical stability and thus can be a good alternative for the substrate of the fragile commercial SPME fibers. High rigidity and durability, long service life, and high extraction capability are some of the other advantages of the offered fiber.

scholarly journals Pre-Concentration and Determination of Tetracyclines Antibiotics Residues in Water Samples Using RGO/Fe3O4 Nanocomposite as Extraction Sorbent

2021 ◽  
Vol 21 (5) ◽  
pp. 1196
Author(s):  
Ungku Amirul Arif Ungku Abdullah ◽  
Nor Suhaila Mohamad Hanapi ◽  
Wan Nazihah Wan Ibrahim ◽  
Nursyamsyila Mat Hadzir ◽  
Nurzaimah Zaini ◽  
...  
Keyword(s):  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Coefficient Of Determination ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Magnetic Solid

Existing methods used in tracing Tetracyclines' antibiotics (TCAs) residues which pose serious environmental problems, consume high amounts of organic solvents, are time-consuming, and are relatively expensive. A simple and effective magnetic solid-phase extraction (MSPE) based on reduced graphene oxide/magnetite (RGO/Fe3O4) nanocomposite sorbent was successfully developed for preconcentration and extraction of TCAs residues from water samples. The analytes were determined by high-performance liquid chromatography with a diode-array detector (HPLC-DAD). The synthesized nanocomposite was characterized using Fourier-transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD), and field emission scanning electron microscopy (FESEM). Sample pH, amount of adsorbent, sample volume, extraction time, desorption time, and desorption solvent were evaluated and optimized. Under optimized conditions, the method demonstrated good linearity over the concentration range of 0.05–1.0 mg L–1 with the coefficient of determination (R2) ≥ 0.9978. Limit of detection (LOD) and limit of quantification (LOQ) were 0.006–0.011 mg L–1 and 0.019–0.036 mg L–1, respectively. The accuracy and precision of the developed method were proven by good analyte recovery (89.77–106.33%) and acceptable precision with relative standard deviation, RSD ≤ 5.54%. The results showed that magnetic solid RGO/Fe3O4 could be a suitable adsorbent in the preconcentration and extraction of TCAs in water samples.

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 Development of an analytical method for dibutyl phthalate (DBP) determination in water samples using gas chromatography

2018 ◽  
Vol 44 ◽  
pp. 00200
Author(s):  
Sabina Ziembowicz ◽  
Małgorzata Kida ◽  
Piotr Koszelnik
Keyword(s):  
Gas Chromatography ◽  
Dibutyl Phthalate ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Limit Of Quantification ◽  
Extraction And Separation ◽  
Analytical Curve ◽  
Relative Standard ◽  
Selection Of

The aim of the work described here was to develop and validate a method by which dibutyl phthalate may be subject to determinations using solid phase extraction and gas chromatography. Optimization of the chromatographic method was based on the selection of working conditions for both the chromatograph and the detector. Following the optimization of extraction and separation parameters, the method was validated by evaluating specificity, the analytical curve, linearity, limits of detection and quantification and recovery. The proposed method has been evaluated in terms of linearity, over a range of concentrations from 0 to 7.5 mg·L-1.The analytical curves show values for correlation coefficients higher than 0.99. Mean recoveries from samples ranged from 97 to 127%, with relative standard deviation lower than 11%. Limit of detection LOD and limit of quantification LOQ values were 0.02 and 0.053 mg·L-1 respectively.

scholarly journals Solid Phase Extraction Method for the Determination of Atrazine and Cyanazine in Water Samples

2021 ◽  
Vol 14 ◽  
pp. 1-6
Author(s):  
Nurul Auni Zainal Abidin ◽  
Nur Sofiah Abu Kassim ◽  
Noor Hidayah Pungot
Keyword(s):  
Solid Phase Extraction ◽  
Water Samples ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Water System ◽  
Phase Extraction ◽  
Triazine Herbicides ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Spe Method

Triazine is one of the herbicides group that is widely used in agriculture that acts as an inhibitor for the growth of unwanted weeds in plants. The use of this herbicide on plants is absorbed by the soil and flows into a nearby water system. This research focused on two types of triazines, namely atrazine and cyanazine. This research aims to extract this type of triazine herbicides and to determine their concentration in water samples. It was quantified by using gas chromatography-electron capture detector (GC-ECD). Solid phase extraction (SPE) method was applied to extract herbicides from water samples. The results indicate that all the samples contained atrazine and cyanazine. Studies in the range of 0.5 - 25 mg/L achieved good linearity with good correlation of determination, r2 value of 0.9922 - 0.9982 mg/L. Relative standard deviations (RSD) for triplicate analysis of the samples were less than 10.0%. The limit of detection (LODs) and limit of quantification (LOQs) of cyanazine and atrazine were found, ranging from 3.33 – 6.67 μg/L and 11.09 – 20.10 μg/L, respectively. The recoveries of the triazine herbicides studied in water samples ranged from 82.5% to 107.6%. The developed method exhibited excellent clean-up capability and was successfully applied for determining triazine herbicide residues in water samples.

Determination of Major Phytohormones in Fourteen Different Seaweeds Utilizing SPE–LC–MS/MS

2019 ◽  
Vol 58 (2) ◽  
pp. 98-108 ◽  
Author(s):  
Sibel Yalçın ◽  
Emine Şükran Okudan ◽  
Özge Karakaş ◽  
Ayşe Nur Önem
Keyword(s):  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Tandem Mass ◽  
Mass Detection ◽  
Hydrophilic Lipophilic Balance ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

Abstract Analysis of plant growth regulators (PGRs) should be approached by considering their extremely low concentrations and serious interfering effects that result from the matrix of various plant tissues. In the current research, the separation and simultaneous determination of different classes of phytohormones in 14 seaweeds collected from Turkey seashores were achieved by using solid-phase extraction (SPE) followed by a rapid and sensitive liquid chromatography tandem mass detection method. OASIS HLB (Hydrophilic-Lipophilic Balance) cartridges were successfully used for SPE process to eliminate the matrix effect and enhance the PGRs including zeatin, benzyl amino purine, indole-3-acetic acid, abscisic acid and gibberellic acid within partially different polarities. Based on the optimized experimental conditions, the method presented excellent performance related to linearity (r, 0.9996–0.9999) within the ranges of 0.5–500 ng/mL, relative standard deviation values ((1.43–2.01) for intraday and (2.36–3.50) for interday)), the limit of detection (0.01–0.84 μg/L) and the limit of quantification (0.02–2.76 μg/L). The obtained results confirm that the SPE–liquid chromatography/tandem mass spectrometry method performed is highly effective and convenient for routine analyses of trace amounts of the tested phytohormones in seaweeds and any other plant samples as well.

Factorial Design Optimisation of Solid Phase Extraction for Preconcentration of Parabens in Wastewater Using Ultra-High Performance Liquid Chromatography Triple Quadrupole Mass Spectrometry

2020 ◽  
Vol 16 (4) ◽  
pp. 436-446
Author(s):  
Vallerie A. Muckoya ◽  
Philiswa N. Nomngongo ◽  
Jane C. Ngila
Keyword(s):  
Solid Phase Extraction ◽  
Formic Acid ◽  
Factorial Design ◽  
Solid Phase ◽  
Treatment Plant ◽  
Phase Extraction ◽  
Limit Of Quantification ◽  
Analytical Technique ◽  
Relative Standard ◽  
Simulated Wastewater

Background: Parabens are synthetic esters used extensively as preservatives and/or bactericides in personal care personal products. Objective: Development and validation of a novel robust chemometric assisted analytical technique with superior analytical performances for the determination of ethylparaben, methylparaben and propylparaben, using simulated wastewater matrix. Methods: An automated Solid Phase Extraction (SPE) method coupled with liquid chromatographymass spectrometry was applied in this study. A gradient elution programme comprising of 0.1% formic acid in deionised water (A) and 0.1% formic acid in Methanol (B) was employed on a 100 x 2.1 mm, 3.0 μm a particle size biphenyl column. Two-level (2k) full factorial design coupled with response surface methodology was used for optimisation and investigation of SPE experimental variables that had the most significant outcome of the analytical response. Results: According to the analysis of variance (ANOVA), sample pH and eluent volume were statistically the most significant parameters. The method developed was validated for accuracy, precision, Limits of Detection (LOD) and Limit of Quantification (LOQ) and linearity. The LOD and LOQ established under those optimised conditions varied between 0.04-0.12 μgL−1 and 0.14-0.40 μgL−1 respectively. The use of matrix-matched external calibration provided extraction recoveries between 78-128% with relative standard deviations at 2-11% for two spike levels (10 and 100 μgL-1) in three different water matrices (simulated wastewater, influent and effluent water). Conclusion: The newly developed method was applied successfully to the analyses of parabens in wastewater samples at different sampling points of a wastewater treatment plant, revealing concentrations of up to 3 μgL−1.

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