Determination of the Residue Behavior and Risk Assessment of Chlorfluazuron in Chinese Cabbage, Kale, Lettuce and Cauliflower by UPLC-MS/MS

Chlorfluazuron is used as a highly effective insect growth regulator to control a variety of crop pests. However, residues of this pesticide have been shown to be harmful to human health. To evaluate the residual dissipation pattern and risk for dietary intake of chlorfluazuron in various vegetables, a solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry method was established to analyze chlorfluazuron residues in Chinese cabbage, Chinese kale, Chinese lettuce, and cauliflower. The sample was extracted with acetonitrile and purified using an SPE amino column. The average recovery of the target sample in the analyzed four vegetables was between 75.0% and 104.1%, and the relative standard deviation was between 2.5% and 9.6%. The precision and accuracy of the analysis met the requirements of residue analysis standards. Dissipation kinetic testing of chlorfluazuron in different vegetables showed a half-life of 2.4–12.6 days, with a rapid dissipation rate. The estimated daily intake of the chlorfluazuron was 0.753–1.661 μg/(kg bw·d), and the risk quotient was 0.15–0.35. It showed that chlorfluazuron had a low risk of chronic dietary intake from vegetables in different populations in China. The results of this study has described the degradation rate of chlorfluazuron in four vegetables, evaluated the risk of dietary exposure to Chinese residents. Therefore, it provides supporting data and empirical basis for guiding the reasonable use of chlorfluazuron in vegetable production and in evaluating its dietary intake risk in vegetables.

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Determination of Imidacloprid, Acetamiprid, Thiabendazole and Carbendazim Residues in Edible Fungi by HPLC

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.781-784.99 ◽

2013 ◽

Vol 781-784 ◽

pp. 99-103 ◽

Cited By ~ 2

Author(s):

Ling Lin ◽

Chun Liang Yang ◽

Zheng Peng ◽

Ming Yue Wang ◽

Zong Qiang Zeng ◽

...

Keyword(s):

Solid Phase ◽

Residue Analysis ◽

Correlation Coefficients ◽

Edible Fungi ◽

Extraction Solvent ◽

Solid Phase Extraction Cartridge ◽

Accuracy And Precision ◽

Relative Standard ◽

Straw Mushroom

A method was developed for simultaneous determination of imidacloprid,acetamiprid, thiabendazole and carbendazim in lentinus edodes, straw mushroom and oyster mushroom by HPLC. Acetonitrile was edded in the sample for extraction solvent, the sample was purified by NH2 solid phase extraction cartridge,then detected by HPLC.The results showed that a good linearity in the range of 0.05~5.0μg/mL with the linear correlation coefficients of 0.9991~0.9997, the detection limits of imidacloprid, acetamiprid, thiabendazole and carbendazim were respectively 0.002 mg/kg,0.005mg/kg, 0.003 mg/kg and 0.003 mg/kg.Tests for recovery were made by addition of four pesticidess standards at three different concentration levels (0.1, 0.5 and 1.0 mg/kg) to the blank sample.The mean recovery rates were 86.0%~105.0% , the relative standard deviations were less than 3.5%.The sensitivity, accuracy and precision of this method were able to meet the requirements for pesticide residue analysis.

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Residue analysis of fosthiazate in cucumber and soil by QuEChERS and GC-MS

Chemical Papers ◽

10.2478/s11696-014-0589-8 ◽

2014 ◽

Vol 68 (10) ◽

Cited By ~ 5

Author(s):

Min Wu ◽

Jiye Hu

Keyword(s):

Solid Phase ◽

Residue Analysis ◽

Field Trials ◽

Residue Level ◽

Gas Chromatography Mass Spectrometry ◽

Dispersive Solid Phase Extraction ◽

First Order ◽

First Order Kinetics ◽

Maximum Residue Level ◽

Relative Standard

AbstractA convenient method was developed for the determination and validation of fosthiazate in cucumber and soil. The procedure is based on liquid partitioning with acetonitrile followed by dispersive solid phase extraction as the clean-up step, after which samples were analysed by gas chromatography-mass spectrometry (GC-MS). The average recoveries ranged from 91.2 % to 99.0 % with relative standard deviations (RSDs) of less than 6.05 %, at three fortification levels (0.02 mg kg−1, 0.1 mg kg−1, 0.5 mg kg−1) in cucumber and soil, and the limits of quantification (LOQs) for fosthiazate were all established at 0.02 mg kg−1. The proposed method was applied successfully to analyses of the dissipation and residue of fosthiazate in field trials. The dissipation rate of fosthiazate was described using pseudo-first-order kinetics with a half-life of 4.33 days and 4.08 days in soil in Beijing and Shandong, respectively. In the terminal residue experiment, fosthiazate residues in cucumber and soil were clearly below the maximum residue level (MRL, 0.2 mg kg−1) set in China.

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Detection, Risk Assessment, and Survey of Four Polycyclic Aromatic Hydrocarbon Markers in Infant Formula Powder

Journal of Food Quality ◽

10.1155/2020/2959532 ◽

2020 ◽

Vol 2020 ◽

pp. 1-9 ◽

Cited By ~ 1

Author(s):

Chenggang Cai ◽

Pinggu Wu ◽

Pingping Zhou ◽

Dajin Yang ◽

Zhengyan Hu

Keyword(s):

Polycyclic Aromatic Hydrocarbon ◽

Aromatic Hydrocarbon ◽

Infant Formula ◽

Solid Phase ◽

Daily Intake ◽

Milk Powder ◽

Internal Standard ◽

Infant Exposure ◽

Relative Standard ◽

Polycyclic Aromatic

A gas chromatography-mass spectroscopy (GC-MS) method was developed to assess the infant exposure assessment from four important polycyclic aromatic hydrocarbon (PAH) markers in infant formula powder: benzo[a]anthracene, chrysene, benzo[b]fluoranthene, and benzo[a]pyrene (collectively referred to as PAH4). The developed method required the addition of an isotopically labeled internal standard, sample extraction under alkali conditions, a saponification step, and a solid-phase extraction purification step. In a controlled spike test, the average recovery rates of PAH4 were 77.3% to 111.8% and the relative standard deviations were 4.8% to 14.2% (n = 6). The quantitative limit (LOQ) and detection limit (LOD) of the method were 0.5 and 0.1 μg·kg−1, respectively. The PAH4 content was analyzed in 30 commercially available infant formula powders. The PAH4 content was found to be in the range of 0.1 to 0.87 μg·kg−1. Combined with the daily intake of infant milk powder in China, the average and maximum daily exposure of BaP for stage-1 infants in China are 0.45 ng/kg.bw.d−1 and 1.9 ng/kg.bw.d−1 and the PAH4 values are 8.6 ng/kg.bw.d−1 and 18.6 ng/kg.bw.d−1, respectively. The PAH4 content in the tested infant formula powders sold in the China were sufficiently low, and all of the tested products were safe for consumption.

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The intake of phosphorus through meat products: a health risk assessment

IOP Conference Series Earth and Environmental Science ◽

10.1088/1755-1315/854/1/012057 ◽

2021 ◽

Vol 854 (1) ◽

pp. 012057

Author(s):

D Milicevic ◽

D Vranic ◽

V Koricanac ◽

Z Petrovic ◽

A Bajcic ◽

...

Keyword(s):

Dietary Intake ◽

Adult Population ◽

Daily Intake ◽

Meat Products ◽

Dietary Exposure ◽

Phosphorus Concentration ◽

Acceptable Daily Intake ◽

Retail Markets ◽

Consumption Data ◽

The Mean

Abstract The aim of this study was to assess the dietary exposure of phosphorus in the Serbian adult population by combining individual consumption data with available data for analysed meat products. During a three years period of investigation (2018 to 2020), a total of 682 samples consisting of 425 cooked sausages and 257 smoked meat products were collected from different local retail markets across the Serbia to examine phosphorus concentrations. The mean phosphorus concentration, expressed as P2O5, varied from 4.68±0.88 g/kg to 6.05±1.30 g/kg in finely minced cooked sausages and smoked meat products, respectively. The average estimated daily dietary intake (exposure) (EDI) of phosphorus ranged from 1.115 mg/kg BW (body weight)/day (finely minced cooked sausages) to 1.441 mg/kg BW/day (smoked meat products). Phosphorus dietary intake (exposure) averaged 3.08% of the acceptable daily intake (ADI: 40 mg/kg BW/day). According to our results, the average phosphorus exposure in the Serbian adult population from consumption of these meat products is far below the European ADI.

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Determination of Trace Zearalenone and Its Metabolites in Human Serum by a High-Throughput UPLC-MS/MS Analysis

Applied Sciences ◽

10.3390/app9040741 ◽

2019 ◽

Vol 9 (4) ◽

pp. 741 ◽

Cited By ~ 2

Author(s):

Danlei Sun ◽

Chenglong Li ◽

Shuang Zhou ◽

Yunfeng Zhao ◽

Yun Gong ◽

...

Keyword(s):

Human Serum ◽

High Throughput ◽

Solid Phase ◽

Internal Standard ◽

Ultra Performance Liquid Chromatography ◽

Enzyme Hydrolysis ◽

Serum Samples ◽

Relative Standard ◽

Before And After

This paper described an improved method for high-throughput and sensitive determination of zearalenone and its five metabolites (zearalanone, α-zearalenol, β-zearalenol, α-zearalanol and β-zearalanol) in human serum. Serum samples were measured both before and after enzyme hydrolysis to assess the free and total amount of each compound by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) in multi reaction monitoring (MRM) mode following off-line 96-well μElution solid-phase extraction (SPE). All the analytes were completely separated on a C18 column within 6 min. It enabled multi-sample preparation at the same time eliminating tedious evaporation and reconstitution steps, allowing 96 (one plate) samples to be processed and analyzed within 24 h. Using an isotope labelled internal standard (13C-ZEN), high recoveries were achieved for all the compounds in the range 91.6%–119.5%, with intra-day and inter-day relative standard deviations (RSDs) of less than 8%. The limits of detection (LOD) and the limits of quantification (LOQ) were 0.02–0.06 ng mL−1 (0.6–2 fmol) and 0.1–0.2 ng mL−1 (3–6 fmol), respectively, demonstrating a notable enhancement in sensitivity compared to the existing methods. The validated method was applied to the analysis of paired urine and serum samples collected from 125 healthy individuals in Henan Province, locating in the middle area of China. ZEN metabolites in human serum were significantly lower than those in urine. Only one serum sample was positive for ZEN after enzyme digestion, whereas at least one of ZEN biomarkers was detected in 75.2% of the paired urine samples. Some comparison and discussion were also included in this paper.

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Dissipation Dynamics and Dietary Risk Assessment of Kresoxim-Methyl Residue in Rice

Molecules ◽

10.3390/molecules24040692 ◽

2019 ◽

Vol 24 (4) ◽

pp. 692

Author(s):

MingNa Sun ◽

Lu Yu ◽

Zhou Tong ◽

Xu Dong ◽

Yue Chu ◽

...

Keyword(s):

Risk Assessment ◽

Dietary Intake ◽

High Efficiency ◽

Dynamic Testing ◽

Residue Analysis ◽

Daily Intake ◽

Brown Rice ◽

Rice Plants ◽

Dietary Risk ◽

Dietary Risk Assessment

Kresoxim-methyl is a high-efficiency and broad-spectrum fungicide used for the control of rice fungal diseases; however, its residues after application potentially threaten human health. Investigations on the dissipation of kresoxim-methyl residue in rice field systems and dietary risk assessment of kresoxim-methyl in humans are limited. The present study employed the QuEChERS-GC-MS/MS method for residue analysis of kresoxim-methyl in rice plants, brown rice, and rice husks. The samples were extracted with acetonitrile and purified by PSA, C18 column, and GCB. The average recovery of the spiked target compounds in the three matrices was between 80.5% and 99.3%, and the RSD was between 2.1% and 7.1%. The accuracy and precision of the method is in accordance with the requirements of residue analysis methods. Dissipation dynamic testing of kresoxim-methyl in rice plants indicated a half-life within the range of 1.8–6.0 days, and a rapid dissipation rate was detected. Dietary intake risk assessment showed that the national estimated daily intake (NEDI) of kresoxim-methyl in various Chinese subpopulations was 0.022–0.054 μg/(kg bw·days), and the risk quotient (RQ) was 0.0000055–0.00014%. These findings indicate that the risk for chronic dietary intake of kresoxim-methyl in brown rice is relatively low. The present study provides information and theoretical basis for guiding the scientific use of kresoxim-methyl in rice fields and evaluating its dietary risk in brown rice.

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Method Development and Validation for Simultaneous Quantification of Microcystin Congeners in Water

10.21203/rs.3.rs-630260/v1 ◽

2021 ◽

Author(s):

Xiaocui Qiao ◽

Simin Ge ◽

Chengyou Liu ◽

Lixin Jiao ◽

Xue Li ◽

...

Keyword(s):

Formic Acid ◽

Method Development ◽

Limit Of Detection ◽

Solid Phase ◽

Signal To Noise Ratio ◽

Internal Standard ◽

Ultra Performance Liquid Chromatography ◽

Chaohu Lake ◽

Online Spe ◽

Relative Standard

Abstract Background: Microcystins, as secondary metabolites of cyanobacteria, are hepatotoxic to humans through the ingestion of cyanobacteria-contaminated water. Microcystins with diverse congeners in water can be precisely quantified using online solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (online-SPE UPLC-MS/MS). A method was developed and validated to simultaneously quantify eight microcystin congeners in water using online-SPE UPLC-MS/MS.Results: The method achieved the highest efficiency and sensitivity by selecting acetonitrile with 0.1% formic acid and water with 0.1% formic acid as the best mobile phase conditions. Linearity, accuracy, and precision were validated on matrix-mixed water with the leucine enkephalin internal standard. The limit of detection calculated using the signal-to-noise ratio of 3 passed the surface water daily inspection for microcystins. Except for the lower recovery of individual substances at individual concentrations, the recoveries of the remaining microcystin congeners ranged from 70 to 130%, and the relative standard deviation was less than 10%.Conclusion: The method was used to analyze microcystins in 12 water samples collected from Chaohu Lake. The sum of all microcystin congeners ranged from 101 to 585 ng L-1 in water (<WHO drinking water safe limit of 1 μg L-1 for microcystin-LR).

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Chemical Characterization and Quantification of Silver Nanoparticles (Ag-NPs) and Dissolved Ag in Seafood by Single Particle ICP-MS: Assessment of Dietary Exposure

International Journal of Environmental Research and Public Health ◽

10.3390/ijerph18084076 ◽

2021 ◽

Vol 18 (8) ◽

pp. 4076

Author(s):

Alfina Grasso ◽

Margherita Ferrante ◽

Giovanni Arena ◽

Rossella Salemi ◽

Pietro Zuccarello ◽

...

Keyword(s):

Silver Nanoparticles ◽

Dietary Intake ◽

Single Particle ◽

Unsaturated Fatty Acids ◽

Daily Intake ◽

Chemical Characterization ◽

Dietary Exposure ◽

In Vivo Studies ◽

Health Concern ◽

Environmental Study

This study provides a first insight on the chemical characterization and quantification of silver nanoparticles (AgNPs) and dissolved Ag in processed canned seafood products, where food-grade edible silver (E174) is not intentionally added nor is the nanoparticle contained in the food contact material. The aim was to evaluate the bioaccumulation potential of AgNPs and to contribute to the assessment of AgNPs and ionic Ag human dietary intake from processed seafood. It is known how seafood, and in particular pelagic fish, is a precious nutritional source of unsaturated fatty acids, protein, and different micronutrients. Nevertheless, it may cause possible health problems due to the intake of toxic compounds coming from environmental pollution. Among emerging contaminants, AgNPs are widely applied in several fields such as biomedicine, pharmaceutical, food industry, health care, drug-gene delivery, environmental study, water treatments, and many others, although its primary application is in accordance with its antimicrobial property. As a consequence, AgNPs are discharged into the aquatic environment, where the colloidal stability of these NPs is altered by chemical and physical environmental parameters. Its toxicity was demonstrated in in-vitro and in-vivo studies, although some findings are controversial because toxicity depends by several factors such as size, concentration, chemical composition, surface charge, Ag+ ions released, and hydrophobicity. The new emerging technique called single-particle inductively coupled plasma mass spectrometry (spICP-MS) was applied, which allows the determination of nanoparticle number-based concentration and size distribution, as well as the dissolved element. Our findings highlighted comparable mean sizes across all species analysed, although AgNPs concentrations partly follow a trophic level-dependent trend. The low mean size detected could be of human health concern, since, smaller is the diameter higher is the toxicity. Dietary intake from a meal calculated for adults and children seems to be very low. Although seafood consumption represents only a small part of the human total diet, our findings represent a first important step to understand the AgNPs dietary exposure of the human population. Further studies are needed to characterize and quantify AgNPs in a large number of food items, both processing and not, and where AgNPs are added at the industrial level. They will provide a realistic exposure assessment, useful to understand if AgNPs toxicity levels observed in literature are close to those estimable through food consumption and implement data useful for risk assessors in developing AgNPs provisional tolerable daily intake.

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Simultaneous Determination of Tetracylines and Quinolones Antibiotics in Egg by Ultra-Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry

Journal of AOAC International ◽

10.1093/jaoac/91.2.461 ◽

2008 ◽

Vol 91 (2) ◽

pp. 461-468 ◽

Cited By ~ 19

Author(s):

Xiaofei Jia ◽

Bing Shao ◽

Yongning Wu ◽

Yi Yang ◽

Jing Zhang

Keyword(s):

Liquid Chromatography ◽

Solid Phase ◽

Ultra Performance Liquid Chromatography ◽

Ion Source ◽

Tandem Mass ◽

Buffer Solution ◽

Solid Phase Extraction Cartridge ◽

Relative Standard ◽

Oasis Hlb ◽

Tandem Mass Spectrometric

Abstract We report here an ultra-performance liquid chromatography coupled with tandem mass spectrometric (MS/MS) method for the simultaneous quantitation of multiclass veterinary drugs in egg. The analysis of the target compounds, including 7 tetracyclines and 4 types of quinolones, may be accomplished in 15 min of total run time. The egg was extracted with ethylenediaminetetraacetic acidMcIlvaine buffer solution and further purified using a polymer-based Oasis HLB solid-phase extraction cartridge. A C18 column was used to separate the analytes followed by MS/MS using an electrospray ion source. The overall average recoveries of the analytes based on matrix-fortified calibration ranged from 71 to 112 with acceptable relative standard deviations of <20 for 6 trials. For all of the target compounds, the limits of quantitation ranged between 0.02 and 4.29 g/kg. The proposed method is sufficiently sensitive and highly selective.

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Magnetic Polyamide Nanocomposites for the Microextraction of Benzophenones from Water Samples

Molecules ◽

10.3390/molecules24050953 ◽

2019 ◽

Vol 24 (5) ◽

pp. 953 ◽

Cited By ~ 1

Author(s):

Hoda Ghambari ◽

Emilia Reyes-Gallardo ◽

Rafael Lucena ◽

Mohammad Saraji ◽

Soledad Cárdenas

Keyword(s):

Water Samples ◽

Extraction Efficiency ◽

Solid Phase ◽

Ultra Performance Liquid Chromatography ◽

Optimum Conditions ◽

Photodiode Array Detection ◽

Real Water Samples ◽

Relative Standard ◽

Photodiode Array ◽

Array Detection

In this article, the influence of the monomers on the extraction efficiency and the effect of the addition of surfactants during the synthesis have also been considered. The sorption capacity of the resulting nanocomposites has been evaluated, in the dispersive micro-solid phase extraction format, by determining that of six benzophenones in water using ultra performance liquid chromatography (UPLC) combined with photodiode array detection. Under the optimum conditions, the limits of detection were in the range of 0.5–4.3 ng/mL and the repeatability, expressed as the relative standard deviation (RSD), varied between 1.5% and 5.6%. The proposed method has been applied for the analysis of real water samples, providing relative recoveries in the interval of 84–105%

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