Determination of paraquat and diquat: LC-MS method optimization and validation

Pizzutti, Ionara Regina; Vela, Giovana Milagros Espinoza; Kok, Albert; Scholten, Jos; Dias, Jonatan V.; Cardoso, Carmem D.; Concenço, Germani; Vivian, Rafael

doi:10.1016/j.foodchem.2016.04.069

Cited by 80 publications

(33 citation statements)

References 18 publications

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“…With regard to the direct dilution approach, the ratio of wine and water, 1:4, was applied after the optimized protocol, while for the QuEChERS extraction strategy, the parameters were optimized, which referring to Pizzutti et al, 29 including: the initial weight of wine, amount of acetonitrile and MgSO4 used in LLME step, shaking time, centrifuging rate. In this part, we focus on the optimization process of the QuEChERS extraction strategy, using wine number 6 in this experiment.…”

Section: Sample Preparationmentioning

confidence: 99%

Quantification of Trans-resveratrol in Red Wines Using QuEChERS Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry

Liao

Chen

2018

ANAL. SCI.

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Resveratrol is one of representative ingredient in red wine, but its quantification is a challenge because of a complex and abundant matrix. In this study, two sample pretreatments, direct dilution and QuEChERS extraction, coupling LCMS analysis were examined for resveratrol quantification. Similar recoveries of 106.4 to 93.7% were obtained for direct dilution and QuEChERS, respectively. With the aid of condition optimization, QuEChERS extraction could concentrate the resveratrol from red wines to improve the detection sensitivity with a LOD value of 2.5 ng/mL, which is four-times greater than the direct dilution approach. As a result, the QuEChERS method can provide a high linearity within the concentration range of 5 - 500 ng/mL, in which direct dilution produced the linear calibration curve within the concentrations of 25 - 500 ng/mL. A high consistency was obtained for both approaches in which intra-day precisions were within 0.5 to 7.2% (n = 3), and the inter-day precisions were within 7.8 to 16.0% (n = 9). Overall, the sample pretreatment of QuEChERS can effectively reduce the matrix effect, which leads LCMS to quantify the low resveratrol abundance of 8.0 ppb in each red wine sample, which is not achieved with the direct dilution approach.

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Section: Sample Preparationmentioning

confidence: 99%

Quantification of Trans-resveratrol in Red Wines Using QuEChERS Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry

Liao

Chen

2018

ANAL. SCI.

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“…It is, therefore, not amenable to multiresidue extraction by quick, easy, cheap, effective, rugged, and safe (QuEChERS) or similar protocols. This analysis mostly involves single residue methods, where the aqueous or food matrices are extracted with acidified methanol, or acidified water . Recently, the analysis of paraquat residue in various fruit matrix has been reported by Oulkar et al, which involved extraction with acidified water (0.1 m HCl) at 80 °C (15 min), followed by LC‐MS/MS analysis involving hydrophilic interaction liquid chromatography (HILIC).…”

Section: Introductionmentioning

confidence: 99%

Determination of Paraquat Residues in Palm Oil by High‐Performance Liquid Chromatography with UV and Tandem Mass Spectrometry

Halim

Kuntom

Shinde

et al. 2019

Euro J Lipid Sci & Tech

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This paper describes a method for determination of paraquat residues in palm oil products by liquid chromatography with ultraviolet detector (HPLC‐UV) and liquid chromatography with tandem mass spectrometry (LC‐MS/MS). The sample (5 g) is extracted with 10 mL ethyl acetate/deionized water and purified through a Strata X‐CW anion exchange solid‐phase extraction (SPE) cartridge. While using HPLC, the chromatographic separation is carried out using a reverse phase pentafluorophenyl column with the mobile phase comprising 95% water and 5% methanol with 0.2% trifluoroacetic acid (TFA). Analysis on a hydrophilic interaction liquid chromatography (HILIC) column did not require TFA. The limits of detection (LOD) and quantification (LOQ) for HPLC‐UV analysis are 0.025 μg mL−1 and 0.05 μg mL−1, respectively. The LC‐MS/MS method did not require an SPE clean‐up and provided an LOQ of 0.01 μg mL−1. The percentage recoveries at the fortification levels of 0.1, 0.05, and 0.01 mg kg−1 are between 70 and 120% with the precision RSD <20%. The matrix effects in LC‐MS/MS analysis are from 40 and 65%, while the recoveries are corrected by paraquat‐D6 as an internal standard. The optimized and validated method fulfills the criteria of DG‐SANTE guidelines and complied with the MRL requirements. Practical Applications: A simple method is reported for the quantitative analysis of paraquat in palm oil products by using HPLC equipped with UV and MS/MS detections. The optimized method fulfills the Codex guidelines on performance criteria for methods of analysis for the determination of pesticide residues in food and feed requirements and meet the Codex maximum residue level (CODEX MRL) in terms of analytical sensitivity and passed all criteria of European Commission's DG‐SANTE guideline (SANTE/11813/2017) of analytical quality control. The method will be useful for regulatory enforcement as well as high throughput commercial residue testing purposes. An efficient residue analysis method is reported for determination of paraquat in palm oil by HPLC‐UV and LC‐MS/MS techniques. The optimized method provides acceptable performance in terms of recoveries and precision as per the SANTE/11813/2017 guideline. The method sensitivity complies with the Codex MRL. The method is suitable for monitoring and enforcement of paraquat residues in a range of palm oil products. It holds promise for routine use in regulatory as well as commercial residue testing laboratories.

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“…The ingestion of the most toxic quats, PQs, into the human body can have long-term health effects, such as Parkinson's disease, liver failure, heart failure, lung damage, and skin cancer [6]. Therefore, it has been banned in some countries [7,8]. Chromatographic techniques, such as gas chromatography (GC) and high performance liquid chromatography (HPLC), have been used as powerful techniques for simultaneous analysis of quats [9][10][11][12][13].…”

Section: Introductionmentioning

confidence: 99%

Supramolecular Solvent-Based Liquid Phase Microextraction Combined with Ion-Pairing Reversed-Phase HPLC for the Determination of Quats in Vegetable Samples

Hem¹,

Gissawong²,

Srijaranai³

et al. 2019

Toxics

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In this study, we used anion supramolecular solvent (SUPRAS) prepared from a mixture of an anionic surfactant, sodium dodecyl sulfate (SDS), and a cationic surfactant, tetrabutylammonium bromide (TBABr), as the extraction solvent in liquid phase microextraction (LPME) of paraquat (PQ) and diquat (DQ). The enriched PQ and DQ in the SUPRAS phase were simultaneously analyzed by ion-pairing reversed-phase high performance liquid chromatography. PQ and DQ were successfully extracted by LPME via electrostatic interaction between the positive charge of the quats and the negative charge of SUPRAS. PQ, DQ, and ethyl viologen (the internal standard) were separated within 15 min on a C18 column, with the mobile phase containing 1-dodecanesulfonic acid and triethylamine, via UV detection. The optimized conditions for the extraction of 10 mL aqueous solution are 50 μL of SUPRAS prepared from a mixture of SDS and TBABr at a mole ratio of 1:0.5, vortexed for 10 s at 1800 rpm, and centrifugation for 1 min at 3500 rpm. The obtained enrichment factors were 22 and 26 with limits of detection of 1.5 and 2.8 µg L−1 for DQ and PQ, respectively. The precision was good with relative standard deviations less than 3.86%. The proposed method was successfully applied for the determination of PQ and DQ in vegetable samples and recoveries were found in the range of 75.0% to 106.7%.

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Determination of paraquat and diquat: LC-MS method optimization and validation

Cited by 80 publications

References 18 publications

Quantification of Trans-resveratrol in Red Wines Using QuEChERS Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry

Quantification of Trans-resveratrol in Red Wines Using QuEChERS Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry

Determination of Paraquat Residues in Palm Oil by High‐Performance Liquid Chromatography with UV and Tandem Mass Spectrometry

Supramolecular Solvent-Based Liquid Phase Microextraction Combined with Ion-Pairing Reversed-Phase HPLC for the Determination of Quats in Vegetable Samples

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