An efficient and modified Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection were evaluated for the analysis of residues of 72 pesticides in brown rice including acidic sulfonylurea herbicides. For extraction of pesticides and clean-up of the extract, 1% formic acid in acetonitrile and dispersive solid phase extraction were used, respectively. Two fortified spikes at 50 and 200 µg L -1 levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 90 to 110% with standard error (Coefficient of Variation) less than 10%. The limits of detection and quantification ranged from 0.24 to 19.92 µg L -1 and 0.79 to 65.74 µg L -1 , respectively. Good linearity of calibration curves were achieved with R 2 > 0.9943 within the observed concentration range (from 20 to 400 µg L -1 ). The modified method also provided satisfactory results for sulfonylurea herbicides, which could not be determined properly with previously reported methods. This method was applied to determine residues of target pesticides in real samples. A total of 22 pesticides in 31 out of 40 tested samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg L -1 . This pesticide found in two brown rice samples exceeded its MRL regulated for rice in Republic of Korea. Except this pesticide, concentrations of all observed pesticides were lower than their MRLs. The results reveal that the method is applicable for routine analysis of residues of target pesticides in brown rice.
QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/ NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.
Association of official agricultural chemists official method was adapted and used to develop analytical method for determination of 76 pesticides residues in persimmon, grape, and pear by concurrent use of liquid chromatography-tandem mass spectrometry. Despite few exceptions in particular matrix, two fortified spiking (100 and 400 ppb) in three matrices gave satisfactory results in terms of accuracy, repeatability, precision, and linearity. Method detection limits (MDLs) were determined using five low spiking and eight replicate samples. MDLs were calculated by multiplying the standard deviation with student t-value 2.998 for n-1 (7) degree of freedom at 99% confident level. limit of quantification were obtained by multiplying standard deviation with 10. Experimental results indicate grape was the most problematic matrix among tested fruits and persimmon the least. Etoxazole is the most problematic pesticide and not applicable in this method. Developed method was successfully applied for the determination of residual pesticides in blindincurred samples.
As increasing the use of pesticides both in number and amount to boost crop production, consumer concerns over food quality and safety with respect to residual pesticides are also continuously increasing. However, there is still lacking of information that can effectively help to remove residual pesticides in foods. In recent years, contaminant removal by gas (or) glow discharge plasma (GDP) attracts great interests on environmental scientists because of its high removal efficiency and environmental compatibility. It was shown to be effective for the removal of some organophosphorus pesticides, phenols, benzoic acid, dyes, and nitrobenzene on solid substrate or in aqueous solution. This work mainly focuses on the removal of wide range of residual pesticides from fresh fruits and vegetables. As for preliminary study, the experiments were carried out to investigate whether GDP can be used as an effective tool for degrading target pesticides or not. With this objective, 60 selected pesticides drop wised onto glass slides were exposed to two types of GDP, dielectric barrier discharge plasma (DBDP) and low pressure discharge plasma (LPDP), for 5 min. Then, they were washed with 2 mL MeCN which were collected and used for determination of remaining concentration of pesticides using LC-MS/MS. Among selected pesticides, degradation of 18 pesticides (endosulfan-total was counted as one pesticide) by GDP could not be examined because control treatments, which were left in ambient environment, of those pesticides recovered less than 70% or even did not recover. However, majority of tested pesticides (42) were degraded by both types of GDP with satisfactory recovery (>80%) of control sample. Pesticides degradation ranged from 66.88% to 100% were achieved by both types of plasma except clothianidin which degradation in LPDP was 26.9%. The results clearly indicate that both types of gas discharge plasma are promising tools for degrading wide range of pesticides on glass substrate.
In analyzing pesticide residue, LLE (liquid liquid extraction) is generally applied as one of the existing methods, but needed quite a lot of organic solvents and analytical apparatuses for the sample pre-treatment. In addition to its long analysis time and complex analytical processes, it is required to develop a more rapid and efficient method at present. In order to establish an economic and simple pesticide residue analytical method, this study carried out a comparative experiment on the existing analytical method with a new sample pre-treatment method named QuEChERS (quick, easy, cheap, effective, rugged and safe), which extracts and refines pesticide components by directly adding solid powder into the sample. Both the two analytical methods showed favorable values of correlation coefficient (R 2 > 0.99) of calibration curves. In terms of the detection limit (identification limit), imidacloprid showed 0.02 mg/kg, while the rest of pesticides showed a level around 0.05 mg/kg. The results of this experiment revealed that the recovery of LLE was 92.8-100.9% and the RSD was below 2.5%. On the other hand, the recovery of QuEChERS was 92.2-101.6% and RSD was below 1.9%. As a result of comparing the amount of pesticide residue by the time between the two analytical methods by using Paired t-Test, there was no significant difference between the two analytical methods as the p-value ranged from 0.3148-0.9890. Considering the results of the two methods, the QuEChERS method had similar recovery, compared to the analytical method using the existing LLE, and the analytical time was shortened by about one fourth of that of the existing method. Moreover, since it excludes the use of harmful organic solvents like dichloromethane during the process of extraction, thus leading to protecting experimenters health and remarkably reducing the amount of disused solvents, it is judged as an echo-friendly and economic analytical method.
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