Multiresidue determination and potential risks of emerging pesticides in aquatic products from Northeast China by LC-MS/MS.
Fu Lei,Lu Xianbo,Tan Jun,Wang Longxing,Chen Jiping
Journal of environmental sciences (China)
A simple method for determining 33 pesticides with a wide polarity range (logK 0.6-4.5) in aquatic products was developed based on LC-MS/MS. The target analytes included three types of widely used pesticides: insecticides, fungicides and herbicides. Based on the optimization of ultrasonic assisted extraction and GPC clean-up procedures, the matrix effect, extraction recoveries and LOD were improved distinctively. LOQ of this method was below 0.5ng/g for all pesticides, which is superior to values in the literature, and the matrix effect was reduced effectively (-14.7% to 7.5%). The method was successfully applied to investigate the pesticide residue levels of twenty-five samples including seven common kinds of fishes from Northeast China. The results showed that all targeted pesticides were present in the fish samples; however, their levels were low, except for atrazine, linuron, ethoprophos, tetrachlorvinphos, acetochlor and fenthion. Atrazine and linuron caught our attention because the concentrations of atrazine in fish samples from Liaoning province were in the range of 0.5-8ng/g (w/w) with mean concentration of 2.3ng/g, which were far above those of other pesticides. The levels of linuron were in the range of 0.6-6ng/g (mean concentration 2.8ng/g), which were the highest among all targeted pesticides in the Inner Mongolia. This is the first systematic investigation on the characteristics and levels of these pesticides in aquatic products from northeast China. Considering their toxicity and bioaccumulation, the potential risk of atrazine and linuron from consuming aquatic products should be paid more attention.
10.1016/j.jes.2017.09.010
Effect of the various parameters governing solid-phase microextraction for the trace-determination of pesticides in water.
Dugay J,Miège C,Hennion M C
Journal of chromatography. A
The parameters governing solid-phase microextraction (SPME) are investigated, with emphasis on the determination of the partition coefficients, K, and their use to predict the selection of a fibre, depending on the respective characteristics of the fibres and the analytes. Film thickness and stability of the compounds can interfere with the determination of K values. The time profile curves were determined for twelve pesticides having a wide range of water solubilities and polarities and using four fibres (polydimethylsiloxane, polydimethylsiloxane-divinylbenzene, Carbowax-divinylbenzene and polyacrylate). Although the affinity order was different for the four coatings, no correlation was found between the respective characteristics of the fibres and solutes. The two fibres containing divinylbenzene were shown to have the highest affinities and the polydimethylsiloxane had the lowest affinity. The polyacrylate fibre which is the more polar commercial fibre did not provide the highest affinities for the more polar and water-soluble analytes. The important parameters for quantitative analysis have been evaluated. The calibration curves were similar when one analyte of interest was present on its own in a drinking water sample, or when eleven other pesticides were present at the same concentration or when much higher concentrations of other analytes were present in the sample. Linearity was obtained over a wide range of concentrations in drinking water samples. Detection limits are in agreement with European regulatory levels in drinking water for most of the analytes using solid-phase microextraction-gas chromatography-nitrogen-phosphorus detection (SPME-GC-NPD). In contaminated surface water samples, the chromatograms are relatively clean and most of the compounds can be detected at levels lower than 0.5 microgram/l.
10.1016/s0021-9673(97)01036-4
Multiresidue analysis of pesticides with hydrolyzable functionality in cooked vegetables by liquid chromatography tandem mass spectrometry.
Lee Sung Joong,Park Semin,Choi Jin Young,Shim Jae-Han,Shin Eun-Ho,Choi Jeong-Heui,Kim Soo Taek,Abd El-Aty A M,Jin Jong Sung,Bae Dong Won,Shin Sung Chul
Biomedical chromatography : BMC
It would be preferable for pesticide residues substituted by hydrolyzable functionality to be analyzed after cooking because their structures are apt to degrade during boiling and/or heating. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantitative determination of 44 pesticide residues with hydrolyzable functional group in five typical vegetable widely consumed in Republic of Korea is described. The sample clean-up was carried out according to the method of Food Code No. 83 established by the Korea Food and Drug Administration (KFDA). Zorbox XDB-C(18) column was selected for the analysis because of the best peak separation. The LC mobile phase consisted of water and 5 mm methanolic ammonium formate, which resulted in a peak shape with good symmetry at each run. Tandem mass spectroscopic (MS/MS) experiments were performed in ESI positive mode and the multiple reaction monitoring modes. A conventional matrix effect was modified to more comprehensive form 100gamma(ij) (%). A high matrix effect (<-30%) was detected for the seven polar pesticides, namely thiamethoxam, clothianidin, acetamiprid, aldicarb, thiacloprid, pirimicarb and methabenzthiazuron. The limits of detection were in the range of 0.1-8.1 microg/kg, indicating a good sensitivity. Most of the recoveries ranged from 70 to 131% with RSDs <or= 20%. The current method allowed rapid quantitation and identification of low pesticide levels in the cooked vegetable samples. Of the screened pesticide residues, only fluquinconazole and dimethomorph below the maximum residue levels established by the KFDA were detected in onion and cucumber samples.
10.1002/bmc.1176
Experimental design in pesticide extraction methods: A review.
Narenderan S T,Meyyanathan S N,Karri Veera Venkata Satyanarayana Reddy
Food chemistry
The sample extraction process is considered as the essential step in the pesticide residue analysis, as it provides the base for the detection of the pesticides in trace level. Various factors need to be optimized during the extraction of pesticides due to the complexity of the matrix which is time-consuming and tedious. Therefore, the use of experimental design in the optimization process proves to be effective with minimum experiments and cost. This paper is aimed to overview the experimental designs that are frequently used for screening (full factorial, fractional factorial, Plackett-Burman Design) and optimizing (central composite design, Box-Behnken design, Taguchi design, Doehlert design, D-optimal design) the most influential factors to provide a sequential understanding of the linear and complex interactions in the pesticide extraction methods. Further, a systematic approach has been discussed about the use of experimental designs in pesticide extraction and also the softwares used for application-oriented readers.
10.1016/j.foodchem.2019.03.045
Occurrence, detection, and dissipation of pesticide residue in plant-derived foodstuff: A state-of-the-art review.
Food chemistry
Pesticides are indispensably essential in agricultural practices. Traditional pesticides and environmentally friendly pesticides both are used to control the damage caused by pests and diseases. Conventional procedures were carried out to detect pesticide residues using chromatography and spectrophotometric techniques. Innovative extractions (micro-extraction) and detection technologies (biosensors, screening cards, etc.) have been developed for faster and more efficient screening of pesticide compounds in plant-derived foodstuffs. The present review summarized the trends of pesticide occurrence in plant-derived foodstuffs, and discussed the advances in pesticides detection. Also, the pesticide dissipation and the mechanism of action are discussed. The extensive literature review demonstrates various techniques already in use or having futuristic potential for detecting and dissipating pesticides in foodstuffs, which can pave the way for future research efforts.
10.1016/j.foodchem.2022.132494
[Simultaneous determination of 21 organophosphrous pesticides in human serum by QuEChERS-gas chromatography-mass spectrometry].
Li X J,He Y X,Zhu B L
Zhonghua lao dong wei sheng zhi ye bing za zhi = Zhonghua laodong weisheng zhiyebing zazhi = Chinese journal of industrial hygiene and occupational diseases
A method for the simultaneous determination of organophosphrous pesticides inhuman serum was developed. Using C18 and PSA as absorbent, 21 organophosphrous pesticides including methamidophos, dichlorvos, acephate, Omethoate, demeton and etc. in human serum were determined by combing QuEChERS with GC-MS, organophosphrous pesticides were qualitatedsimultaneously by retention time and characteristic ions. Their contents were determined by internal standard method of quantitative ions. The linear range was from0to 0.60μg/ml with a good correlation coefficients (r ≥ 0.9961) . The LODs of this methodranged from 0.0009 to 0.0111 μg/ml. The average recoveries of3 organophosphrous pesticides (methamidophos、dichlorvos and acephate) ranged from 71.8%~85.3%, The average recoveries of other 18 organophosphrous pesticidesranged from 82.9%~102.9%. The relative standard deviations were0.8%~7.0%. The convenient operation and versatility of this method are suitable forthe fast screening and accurate detection of 21 organophosphrous pesticides in human serum.
10.3760/cma.j.issn.1001-9391.2018.05.019
Multi-pesticides residue analysis of grains using modified magnetic nanoparticle adsorbent for facile and efficient cleanup.
Liu Zhenzhen,Qi Peipei,Wang Xiangyun,Wang Zhiwei,Xu Xiahong,Chen Wenxue,Wu Liyu,Zhang Hu,Wang Qiang,Wang Xinquan
Food chemistry
A facile, rapid sample pretreatment method was developed based on magnetic nanoparticles for multi-pesticides residue analysis of grains. Magnetite (FeO) nanoparticles modified with 3-(N,N-diethylamino)propyltrimethoxysilane (FeO-PSA) and commercial C18 were selected as the cleanup adsorbents to remove the target interferences of the matrix, such as fatty acids and non-polar compounds. Rice was used as the representative grain sample for method optimization. The amount of FeO-PSA and C18 were systematically investigated for selecting the suitable purification conditions, and the simultaneous determination of 50 pesticides and 8 related metabolites in rice was established by liquid chromatography-tandem mass spectrometry. Under the optimal conditions, the method validation was performed including linearity, sensitivity, matrix effect, recovery and precision, which all satisfy the requirement for pesticides residue analysis. Compared to the conventional QuEChERS method with non-magnetic material as cleanup adsorbent, the present method can save 30% of the pretreatment time, giving the high throughput analysis possible.
10.1016/j.foodchem.2017.03.082