Modified Quick, Easy, Cheap, Effective, Rugged And Safe Extraction Research Articles

Optimization of the QuEChERS extraction method to determine Polycyclic Aromatic Hydrocarbons (PAHs) in powder aerosol particles collected by cyclone

Conventional methods for collecting and extracting aerosol particles are challenging in accurately characterizing particle-bound polycyclic aromatic hydrocarbons (PAHs) contamination and conducting cellular exposure studies. Therefore, developing direct aerosol sample collection and simple pretreatment analytical methods is necessary. This study describes the optimization of the QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction method for the determination of PAHs in powder-form environmental standard materials (SRM1944) and proves it is also effective for analyzing PAHs in powder aerosol particle samples collected by cyclone. In this study, we used an I-optimal design response surface method combined with a desirability function to investigate the extraction effect of PAHs under different combinations of QuEChERS extraction factors, including extraction solvent, salt, and clean-up reagent. The optimized conditions of the method were determined using the 2-factor interaction (2FI) model combined with boundary conditions, resulting in acetonitrile/dichloromethane (7:1, v/v), Na2SO4/NaCl (1:1, w/w), and primary and secondary amine (PSA) as extraction solvents, extraction salts, and clean-up reagent, respectively. The optimized method showed good recoveries of PAHs reaching 76%–118% and 85%–121% for SRM1944 and standard solution. The results for cyclone-collected ambient powder aerosol particles extracted by the optimized QuEChERS illustrated that this improved procedure has good PAHs extraction efficiency as the traditional Soxhlet method, while reducing hazardous organic solvents usage, experimental cost (per mg sample) by 97% and sample pretreatment time. Overall, this combination of “powder aerosol particle collection and modified QuEChERS extraction” provides new insight on aerosol sample collection, extraction, and in vitro/in vivo exposure studies.

Analysis of polychlorinated biphenyls in cream and ice cream using modified QuEChERS extraction and GC‐QqQ‐MS/MS method: A risk assessment study

The concentrations of six non–dioxin‐like polychlorinated biphenyls (NDL‐PCBs) were measured using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) by gas chromatography (GC) coupled with triple‐quadrupole (QqQ) tandem mass spectrometry (MS/MS) method in cream and ice cream offered in Tehran (Iran). The results showed the limits of detection, limit of quantification and recovery for the PCB analytes in the ranges 0.04–0.16, 0.132–0.482 ng/g fat, 5.2–9.2 and 95.5–107.2%, respectively. The results showed the mean concentration of total 6NDL‐PCBs in cream (21.634 ± 2.18 ng/g fat) was higher than that in the ice cream (12.317 ± 1.524 ng/g fat) samples. The estimated daily intake (EDI) was lower than the tolerable daily intake (TDI < 10 ng/kg BW/day). Ultimately, the probabilistic model with Monte Carlo simulation (MCS) revealed the incremental lifetime cancer risk levels (95th) of PCB compounds in ice cream (adults = 1.62E−6 and children = 4.37E−6) and cream (adults = 9.65E−7 and children = 7.57E−6) were lower than the level of acceptable risk (10−4).

A Combination of Chromatography with Tandem Mass Spectrometry Systems (UPLC-MS/MS and GC-MS/MS), Modified QuEChERS Extraction and Mixed-Mode SPE Clean-Up Method for the Analysis of 656 Pesticide Residues in Rice.

The emerging ungovernable application of pesticides in rice farming has attracted public concerns as these hazardous chemicals leave long-lasting environmental impacts and cause severe health effects. Here, an optimized analytical method was proposed for the measurement of 656 pesticide residues in rice samples collected in Vietnam. We utilized chromatography with tandem mass spectrometry systems (UPLC-MS/MS and GC-MS/MS) combined with a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method and adopted a mixed-mode SPE clean-up method for the analysis. The results showed that a total of 341 and 315 compounds were determined by UPLC- and GC-MS/MS, respectively. Usage of 10 mL MeCN, 5 mL H2O and 1% glacial acetic acid as extraction solvent outperformed other mixtures in purifying the analytes from the sample matrix. Besides, pressure swing adsorption connected to a C18 cartridge with C18 placed on top exhibited remarkably more extracted compounds of high recovery which resulted in 299 and 318 compounds with recovery ranging from 70 to 120% in GC- and UPLC-MS/MS, respectively. Our optimized protocols also resulted in maximal limits of quantification of 10 μg Kg−1 in both MS methods with repeatability and reproducibility less than 20%. Application of validated method on 20 rice samples collected in Hanoi, Vietnam showed that 14 samples were contaminated with at least one pesticide, and insecticide was the most detected group. Overall, the compliance of all method validation parameters to SANTE/12682/2019 Guideline demonstrates that this protocol can be employed for the effective management of Vietnam’s rice in accordance with international requirements.

Liquid chromatography-high-resolution mass spectrometry analysis of erectile dysfunction drugs and their analogues in food products

The presence of erectile dysfunction (ED) drugs in adulterated dietary supplements, mainly in pharmaceutical dosage forms, is frequently addressed in the literature. Little attention is given to food products despite their increasing adulteration trend. To address this knowledge gap targeted, suspected-target, and non-targeted strategies were utilised to analyse ED drugs and their analogues in powdered drink mix (PDM), honey, jelly, hard candy, and sugar-coated chewing gum using liquid chromatography-high-resolution mass spectrometry (LC-HRMS). The method was optimised and validated using 23 target analytes, representing different ED drugs with structural similarities. The modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction exhibited insignificant matrix effect (ME) within − 9.2–8.8% and provided complete coverage of target analytes with acceptable extraction recovery (RE) within 75.5–123.9%, except for carbodenafil in the PDM matrix. Based on the ME and RE performance, the analytical method was validated to analyse 25 food samples that claimed to enhance male sexual performance. The method exhibited good specificity and linearity with a limit of detection within 10–70 ng/mL and limit of quantification of 80 ng/mL. Similarly, the accuracy and precision were satisfactory within 77.4–122.0% and< 16.7%RSD, respectively. The LC-HRMS targeted analysis, together with suspected-target and non-targeted screenings, identified and detected ten ED drugs from 24 food samples. The modified QuEChERS extraction with LC-HRMS-based method was demonstrated to be universally applicable to various food products, covering an extensive range of known and potentially novel ED drugs, which is valuable for routine casework.

Multi-detection method for mycotoxins with a modified QuEChERS extraction in feed and development of a simple detoxification procedure

A new multi-mycotoxin analysis method was developed to identify and quantify 22 mycotoxins in multiple feed matrices. This method is based on a QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction procedure followed by the ultra-high liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) detection. The QuEChERS extraction procedure was optimized for minimizing the matrix effect of maize. Obtained recoveries ranged from 67 % to 94 % and low LOQs (from 0.22 to 32.64 μg/kg) for regulated and emerging mycotoxins were obtained. Then, the method was expanded to seven raw materials and eight feedstuffs. In these matrices, the recovery for most mycotoxins was also high enough to fulfill the current legislation. The developed method was used for the analysis of 75 samples obtained from a nearby feed factory. Maize and maize-based products showed the highest occurrence of mycotoxins, although always below the legal limit. In addition, the ability of spheres of different composition and size to eliminate mycotoxins from raw materials and feedstuffs was tested. Up to 28 % of the mycotoxin content can be removed from matrices by using glass spheres of 2 mm of diameter. Therefore, a new process for the physical removal of mycotoxins was developed.

Determination of nine preservatives in processed foods using a modified QuEChERS extraction and quantified by HPLC-PDA

ABSTRACTIn this study, a new method was developed for simultaneously determining nine preservatives, that is, benzoic acid (BA), sorbic acid (SOA), dehydroacetic acid (DHA) and PHBAs (methyl p-hydroxybenzoate [PHBA-me], ethyl p-hydroxybenzoate [PHBA-et], isopropyl p-hydroxybenzoate [PHBA-ipro], propyl p-hydroxybenzoate [PHBA-npro]), isobutyl p-hydroxybenzoate [PHBA-ibut] and butyl p-hydroxybenzoate [PHBA-nbut]), in processed foods, employing liquid chromatography (LC). This procedure accelerated sample preparation and improved efficiency by employing modified quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction without clean-up. Samples were prepared with 20 mL of acetonitrile/water (1:1) with the assistance of a ceramic stone. The extract solutions were diluted 10 times or according to the detection amount and then injected into an LC-PDA. This method showed good linearity, and the LOQs were 10 mg/kg for BA, SOA and DHA and 5 mg/kg for the PHBAs. When validating this method, the recoveries of the nine preservatives were in the range 77.0–99.6%, RSDr values were in the range 0.7–5.3% and those of RSDwr were in the range 2.3–8.4%. These results suggest that this new method is highly reproducible.

Determination of 4(5)-methylimidazole in foods and beverages by modified QuEChERS extraction and liquid chromatography-tandem mass spectrometry analysis

The determination of carcinogenic 4(5)-methylimidazole (4-MeI) in complex matrices at trace levels is a challenge because of its higher polarity and weaker column retention capability. Here, we proposed a novel method for the quantification of 4-MeI in various foods and beverages using modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The evaluated QuEChERS extraction with LC-MS/MS method showed excellent linearity (1–200 μg/L, with correlation coefficient (R2) > 0.999), trueness (91–113%), and precision (relative standard deviation (RSD) ≤ 12.3%), but low matrix effect (92–108%) for cola, tea, beer, coffee beverage, bread, biscuit and instant coffee. The expanded measurement uncertainty was less than 34.4% at 95% confidence level. The proposed method can be successfully applied to determine 4-MeI in 28 commercial foods and beverages purchased from local market. Therefore, we believe this method is likely to provide a potential for 4-MeI determination in practical application.

Determination of multiple organochlorine pesticide residues in shrimp using modified QuEChERS extraction and gas chromatography

Determination of organochlorine pesticide residues in shrimp is very important to ensure the consumer’s safety and to fulfill the importer’s demand. Therefore, a simple and efficient multiple organochlorine pesticide residues analytical method using quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique and Gas Chromatography coupled with Electron Capture Detector (ECD) has been developed and validated for the determination of 19 organochlorine pesticides (α- BHC, δ- BHC, β- BHC, γ- BHC, Heptachlor, Aldrin, Heptachlor Epoxide, γ- Chlordane, α- Chlordane, α- Endosulfan, 4,4 DDE, Dieldrin, Endrin, 4,4 DDD, β- Endosulfan, 4,4 DDT, Endosulfan sulphate, Methoxychlor, and Endrin Ketone) in shrimp. The method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD) and limit of quantification (LOQ). The average recoveries of the selected pesticides ranged from 84% to 106% with RSDr ≤ 14% in four fortification levels of 0.05, 0.1, 0.2 and 0.3 mg kg-1. The linearity was ≥ 0.996 for all of the selected pesticides with matrix matched calibration standards. The LOD ranged from 0.003 to 0.009 mg kg-1 and the LOQ was 0.05 mg kg-1. This method was applied successfully for the residue analysis of 40 shrimp samples collected from different regions in Bangladesh.SAARC J. Agri., 16(1): 81-93 (2018)

Simultaneous Determination of Trace Levels of 12 Steroid Hormones in Soil Using Modified QuEChERS Extraction Followed by Ultra Performance Liquid Chromatography–Tandem Mass Spectrometry (UPLC–MS/MS)

Steroid hormones, mainly secreted by vertebrates, are discharged into the soil environment through surface runoff and land application of animal manure, sewage sludge, and organic fertilizers. The adequate analytical methods for steroid hormones in soil are lacking due to the requirement of rigorous sample pre-treatment. In this study, a rapid and effective modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was developed for trace simultaneous analysis of 12 steroid hormones (estrogen, androgens, and progestogens) in soil samples using ultra performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). Samples were extracted by the mixture of acetonitrile and acetate buffer, and then cleaned with PSA/C18 absorbents. The QuEChERS method was validated by evaluating the linearity, repeatability, accuracy and precision. A suitable linear relationship was obtained in the mass concentration range of 1–100 ng g−1 with high correlation coefficients (> 0.9927). The method enabled the determination of the target analytes with limits of detection between 0.0014 and 0.462 ng g−1 and limits of quantification between 0.0047 and 1.54 ng g−1. Soil was spiked at 5, 50 and 100 ng g−1, and the recoveries ranged from 75.17 to 110.33% with relative standard deviations ≤ 9.45. The developed method was successfully applied to the analysis of soil samples collected in Beijing, and five hormones (E1, E3, αE2, And, and Tes) were detected with the concentrations ranging from 0.35 to 7.09 ng g−1.

A Simple Method for the Determination of Malachite Green and Leucomalachite Green Residues in Fish by a Modified QuEChERS Extraction and LC/MS/MS

A simple method using LC/MS/MS was developed and validated to determine residues of malachite green (MG) and leucomalachite green (LMG) in fish fillet. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique was used to perform the sample preparation. The optimal extraction and cleanup conditions were established using an experimental design. The validation parameters obtained to determine both MG and LMG complied with the requirements established by regulatory agencies for the presence of such substances in fish, which establish that the method must attain, at least, a minimum required performance limit of 2 ng/g. The accuracy values ranged between 95 and 107%, and the precision values were lower than 11.2%. The method was used in the analysis of tilapia samples (n = 20) commercialized in Campinas, SP, Brazil. None of the samples presented detectable levels of MG or LMG residues.

Determination of Multiresidue Pesticides in Green Tea by Using a Modified QuEChERS Extraction and Ion-Trap Gas Chromatography/Mass Spectrometry

The pesticide residues in exported and imported tea products must not exceed the maximum residue limits (MRLs) regulated by the import countries. Tea is a complex matrix that obfuscates the determination of pesticide residues. Many available methods for multiresidue pesticide analysis of tea are time-consuming and require many cleanup steps. The objective of this study was to develop a simple multiresidue method by using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and ion-trap GC/MS/MS, which can identify, confirm, and quantify pesticides in complex matrixes. A tea product was homogenized with water, and the pesticides were extracted with acetonitrile containing 1% acetic acid. The extract was subjected to centrifugation, initial cleanup with dispersive SPE (dSPE), solvent exchange, and final cleanup with dSPE. Diethyl-d10-parathion and triphenyl phosphate were used as the internal standard and surrogate, respectively. The final extract was injected into an ITQ 700 gas chromatograph/mass spectrometer. Quantitation of individual pesticides was based on matrix-matched calibration curves with a correlation coefficient of > 0.9930 for the 22 pesticides selected for the study. The recoveries of the 22 pesticides ranged from 78 to 115%, except those for diazinon (130%) and malathion (122%), with an average RSD of 8.7%. The LOD values of all of the pesticides, except for terbufos, were below the MRLs set by the European Union and Japan.

Rapid determination of phenoxy acid residues in rice by modified QuEChERS extraction and liquid chromatography–tandem mass spectrometry

A new method for the analysis of phenoxy acid herbicide residues in rice, based on the use of liquid extraction/partition and dispersive solid phase extraction (dispersive-SPE) followed by ultra-performance liquid chromatography–electrospray ionization tandem mass spectrometry (UPLC–ESI–MS/MS), is reported. 5% (v/v) formic acid in acetonitrile as the extraction solvent and inclusion of citrate buffer helped partitioning of all the analytes into the acetonitrile phase. The extract was then cleaned up by dispersive-SPE using C18 and alumina neutral as selective sorbents. Further optimization of sample preparation and determination allowed recoveries of between 45 and 104% for all 13 phenoxy acid herbicides with RSD values lower than 13.3% at 5.0 μg kg −1 concentration level. Limit of detections (LODs) of 0.5 μg kg −1 or below were attained for all 13 phenoxy acids. Quantitative analysis was done in the multiple-reaction monitoring (MRM) mode using two combinations of selected precursor ion and product ion transition for each compound. This developed method produced relatively higher recoveries of the acid herbicides with a smaller range of variation and less susceptibility to matrix effects, than the original QuEChERS ( Quick, Easy, Cheap, Effective, Rugged, and Safe ) method.