QuEChERs Combined with Online Interference Trapping LC-MS/MS Method for the Simultaneous Determination of 20 Polyfluoroalkane Substances in Dietary Milk

Yucheng, Yu; Xu, Defeng; Lü, Meiling; Zhou, Shi‐Ping; Peng, Tao; Yue, Zhenfeng; Zhou, Yu

doi:10.1021/acs.jafc.5b00068

Cited by 37 publications

(16 citation statements)

References 33 publications

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“…Electroinactivity of PFAS is the main hindrance to developing electrochemical sensors in which the signal is produced by either direct electron transfer, through oxidation or reduction of the analyte molecule at the surface of the electrode, or an indirect redox reaction with other chemicals in the solution. Therefore, conventional methods to sense trace amounts of PFAS heavily rely on highly sensitive liquid chromatography–mass spectrometry (LC-MS). − However, high cost, long analysis times, and centralized instrumentation limit the use of this method for large-scale sensing applications in the field and the ability to sense contamination at the earliest onset of pollution.…”

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confidence: 99%

Quantifying Interferent Effects on Molecularly Imprinted Polymer Sensors for Per- and Polyfluoroalkyl Substances (PFAS)

2020

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Per- and polyfluoroalkyl substances (PFAS) are emerging as harmful environmental micropollutants. Generally, PFAS species are quantified by mass spectrometry, for which a collected sample is taken to a centralized facility. Robust techniques to quantify PFAS in the field are necessary to diagnose environmental contamination at the earliest onset of pollution. Here, we developed a molecularly imprinted polymer (MIP) electrode for the detection of perfluorooctanesulfonate (PFOS) and explored the MIP surface and the effects of interfering molecules. MIPs were formed by the anodic deposition of o-phenylenediamine (o-PD) in the presence of PFOS template molecules on a glassy carbon macroelectrode. The performance of the resulting MIP electrode was evaluated by the current obtained from the oxidation of ferrocene carboxylic acid as the electrochemical probe. The MIP electrode was able to detect PFOS with a detection limit of 0.05 nM, which is lower than the health advisory limit of 0.14 nM reported by the U.S. EPA. To better understand PFOS association into the MIP, a Langmuir binding model was developed based on the changes in electrochemical responses of the MIP. Fitting the model to the experimental data gave an association constant (K A ) of 4.95 × 1012 over a PFOS concentration range of 0 to 0.05 nM. The binding isotherm of other commonly found substances in contaminated water sources such as chloride, humic acid, perfluorooctanoic acid (PFOA), and perfluorobutanesulfonate (PFBS) was also investigated. In the case of chloride and humic acid, the calculated K A values of 9.05 × 107 and 6.01 × 105, respectively, indicate relatively weak adsorption of these species on the MIP. However, PFOA, which is the carboxylate analog of PFOS, revealed a very close K A value (3.41 × 1012) to PFOS. A greater K A value (1.43 × 1013) was obtained for PFBS, which possesses the same functional group and a smaller molecular size compared to PFOS. The presented platform emphasizes the necessity to develop new strategies to make MIP sensors more specific if practical applications are to be pursued.

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confidence: 99%

Quantifying Interferent Effects on Molecularly Imprinted Polymer Sensors for Per- and Polyfluoroalkyl Substances (PFAS)

2020

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“…Several rigorous protein precipitation steps, lipid hydrolysis and alkaline digestion of milk have been employed as sample pre-treatment techniques to minimize matrix interferences [ 17 , 22 , 23 ]. Nevertheless, these have proven to be tedious, unsafe and expensive and sometimes not necessary, as they usually require large quantities of toxic organic solvents and often lead to losses in analyte recoveries [ 24 , 25 , 26 ].…”

Section: Introductionmentioning

confidence: 99%

“…The quick, easy, cheap, effective, rugged and safe (QuEChERS) method is well known to be accurate and highly productive for the ultra-trace determination of pesticides, veterinary drugs and other organic compounds in food matrices [ 24 ]. The use of this method for the analysis of PFAS in milk and biological samples is yet to be fully demonstrated, however, recent studies [ 24 , 25 , 26 , 28 ] have applied QuEChERS with multiple clean-up stages including the use of dispersive solid extraction (dSPE) and other sorbents, e.g., C18 for the analysis of PFAS. Recently, we reported the application of QuEChERS for the direct analysis of PFAS in dairy milk and infant formula [ 13 ], however, this method needs to be fully validated and extended to other matrices.…”

Section: Introductionmentioning

confidence: 99%

Confirmatory Analysis of Per and Polyfluoroalkyl Substances in Milk and Infant Formula Using UHPLC–MS/MS

2021

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An ultra-high performance liquid chromatography tandem mass spectrometry method was developed and validated for the sensitive determination and unambiguous confirmation of residues of per and polyfluorinated alkyl substances (PFAS) in breastmilk, retail milk and infant formulas following two sample preparation methods. Sample pre-treatment was carried out by a simplified QuEChERS method without requiring dSPE or any further clean-up. The method was validated in accordance with the requirements of Commission Decision 657/2002/EC with slight modifications. The method displayed good linearity with R2 ranging from 0.9843–0.9998 for all target PFAS. The recovery and within-laboratory reproducibility of the method (n = 63) were in the range 60–121% and 5–28%, respectively. The decision limit, detection capability and limit of quantitation ranged from 30–60 ng kg−1 to 40–100 ng kg−1 and 5–50 ng kg−1, respectively. Acceptable matrix effect values in the range −45–29% were obtained with uncertainty of measurement lower than 25% for all target PFAS. The method displays its suitability for the sensitive and high-throughput confirmatory analysis of C4–C14 PFAS in breastmilk, dairy milk and infant formulas.

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“…Nowadays, various analytical methods have been introduced to determine fipronil and its metabolites in diverse matrices such as fruits (Duhan et al,2015), vegetables (Kaur et al, 2015), peanut, soil et al (Li et al, 2015), including gas chromatography (GC) (Guo M et al,2008), GC in tandem with mass spectrometry (GC-MS/MS) (Liu et al, 2019;Ramasubramanian et al, 2014), high performance liquid chromatography (HPLC) (Liu et al, 2008;Neagu et al, 2015), and liquid chromatography in tandem with mass spectrometry (LC-MS/MS) (Raju et al, 2016). Besides, QuEChERS-based method was also applied to determine fipronil in many matrices including eggs (Sack, et al,2011;Xia, et al, 2010), and it was popularized worldwide and proved effective, sensitive and accurate (Aruna et al, 2015;Yu et al, 2015).…”

Section: Introductionmentioning

confidence: 99%

Multi-Residue Analysis of Fipronil and Its Metabolites in Eggs by SinChERS-Based UHPLC-MS/MS

Han¹,

Jin²,

Zhang³

et al. 2021

Food Sci Anim Resour

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A method for simultaneous detection of fipronil (F) and its metabolites fipronil desulfinyl (FD), fipronil sulfide (FS), fipronil sulfone (FSO) in chicken eggs was applied and validated. It includes SinChERS for sample preparation and UHPLC-MS/MS for chemical analysis. Results suggested that formic acid enhanced the recovery of 4 target residues and 1% supplementation to acetonitrile gained higher recoveries than that of 5%. SinChERS integrated extraction and clean-up steps into one, with shorter time (1.5 h) to operate and higher recoveries (97%~100%) than HLB, Envi-Carb-NH2 and QuEChERS, and it consumed the smallest volume of extracting solvent (10 mL) as QuEChERS. Quantitative analyses using external standard method suggested the linear ranges of 4 target compounds were 1~20 µg/L with R 2 >0.9947. The limit of detection (S/N>3) and quantification (S/N>10) were 0.3 μg/kg and 1 μg/kg. Recoveries ranged from 89.0% to 104.4%, and the relative standard deviations (n=6) at 1, 10, 20 μg/kg were lower than 6.03%. Thirty batches of domestic eggs (500 g each) were detected by the established SinChERS-based UHPLC-MS/MS and no target residues were detected in all samples.The method developed in this study is a rapid, sensitive, accurate and economic way for multi-residue analysis of fipronil and its metabolites in eggs.

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QuEChERs Combined with Online Interference Trapping LC-MS/MS Method for the Simultaneous Determination of 20 Polyfluoroalkane Substances in Dietary Milk

Cited by 37 publications

References 33 publications

Quantifying Interferent Effects on Molecularly Imprinted Polymer Sensors for Per- and Polyfluoroalkyl Substances (PFAS)

Quantifying Interferent Effects on Molecularly Imprinted Polymer Sensors for Per- and Polyfluoroalkyl Substances (PFAS)

Confirmatory Analysis of Per and Polyfluoroalkyl Substances in Milk and Infant Formula Using UHPLC–MS/MS

Multi-Residue Analysis of Fipronil and Its Metabolites in Eggs by SinChERS-Based UHPLC-MS/MS

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