Development of a new QuEChERS method based on dry ice for the determination of 168 pesticides in paprika using tandem mass spectrometry
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The pesticides residues in food is an important problem related to food safety.In recent years, QuEChERS-Chromatography Mass Spectrometry,as an efficient technical in Multi-residue Determination of Pesticides,is becoming the focus of study in the world.QuEChERS method has received much concern as a quick,easy,cheap,effective, rugged and safe sample preparation method.Due to its efficient separation and qualitative evaluation capacity,dozens or even more hundreds of complex compounds can be separated,qualitated and quantitated by Chromatography Mass Spectrometry in a short time.This article summarizes the application of QuEChERS-Chromatography Mass Spectrometry in multi-residue determination of pesticides in plant-derived foods and animal-derived foods and forecasts the bright prospect of QuEChERS-Chromatography Mass Spectrometry.
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This article used QuEchERS method,known as to be quick,easy,cheap,effective,rugged and safe,to determinate 11 pesticides residues in vegetables.After extraction and cleanup,the samples were detected by GC/MS.The LOQ and average recovery ratio were 5.6～18.2μg/kg and 67.7%～102.3% respectively,while RSD was less than 10.6%.The results show the QuEchERS method can be used for the determination of organophosphorus pesticide residues in vegetables.
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Three modifications of the QuEChERS (quick, easy, cheap, effective, rugged and safe) method for determination of 35 endocrine disrupting pesticides in samples with high acid content such as lemons were studied. Pesticides extraction was performed using the original QuEChERS method, citrate buffered QuEChERS method (EU version) and acetate buffered QuEChERS method (AOAC version). Final extracts were evaluated by fast gas chromatography-mass spectrometry (GC-MS) analysis. Validation experiments for all three methods were performed using a spiked pesticide free lemon matrix and matrix-matched standard solutions. Four concentration levels (1, 20, 50 and 250 μg kg−1) were tested. Recoveries from 70 to 120% with a relative standard deviation <20% were obtained for the majority of pesticides. Linearity was evaluated at a concentration range of 1–250 μg kg−1 for the buffered QuEChERS (AOAC) method with coefficients of determination (R2) higher than 0.9552 and for the original QuEChERS method with R2 higher than 0.9232. The best linearity was obtained for the citrate buffered method with R2 higher than 0.9656. The limit of detection (LOD) of the buffered QuEChERS (AOAC) method ranged between 0.1 and 18.4 μg kg−1, for the citrate buffered QuEChERS method between 0.1 and 23.6 μg kg−1 and for the original QuEChERS method between 0.1 and 14.2 μg kg−1. Results obtained by the three different QuEChERS methods were compared. The citrate buffered method is more suitable for the tested pesticides than the other two QuEChERS methods. Although the QuEChERS method is widely applied, it was shown that in difficult matrices such as lemons, the choice of modifications is analyte/matrix dependent. The three developed and validated methods were applied to the analysis of real citrus samples.
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The recent trend for pesticide residue analysis in food involves fast cleanup and use of mass spectrometry to achieve quantitative and qualitative analysis at the same time. Recently, the QuEChERS (quick, easy, cheap, effective, rugged and safe) multi-reside method has received much attention as a fast extraction and cleanup method of pesticide residue analysis. Therefore, multi-residue analysis of 236 pesticides was tested with the QuEChERS method by concurrent use of PTV-GCITOFMS (gas chromatographyl time-of-flight mass spectrometry with programmable temperature vaporizer). PTV condition was optimized and when the method was applied to apples, pesticide recovery rates (spiked at 400 ng/g) ranged from 80% to 120%, and RSD values were under 10% for most compounds. The results showed that the QuEChERS sample preparation and PTV -GCITOFMS analysis can be applied to multi-residue analysis of pesticides in fruits and vegetables.
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The presence of the nucleoside antitumor antibiotic toyocamycin in the fermentation broth was determined by a combination of negative and positive ion fast atom bombardment (FAB) mass spectrometry, high resolution FAB mass spectrometry and mass-analysed ion kinetic energy spectrometry (MIKES). A reasonable limit of detection for toyocamycin in the whole broth was obtained by combining the specificity of mass spectrometry/mass spectrometry (also called tandem mass spectrometry) to FAB. The role played by the fermentation matrix upon the production and the observation of characteristic ions by FAB using xenon atoms was examined. High-performance liquid chromatography (HPLC) and FAB mass spectrometry were used to monitor toyocamycin at all stages of strain development, fermentation and recovery.
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QuEChERS(Quick, Easy, Cheap, Effective, Rugged and Safe)분석법은 고체상의 분말을 시료에 직접 주입하여 농약성분을 추출하는 방법으로 분석법이 간단하고 빠르기 때문에 많이 연구되고 있다. 이 방법은 기존 분석법에 비하여 적은 시료량과 상대적으로 많은 불순물을 포함하고 있기 때문에 LC-MS/MS 등의 감도가 높은 분석기기를 필요로 하며, HPLC나 GC 분석을 위해서는 개선이 필요하다. 본 연구에서는 QuEChERS AOAC Official 2007.01 법을 개선하여 사과, 포도, 배, 단감 4가지 과일을 대상으로 UPLC-PDA, GC-${\mu}ECD$ 및 GC-NPD 을 이용하기 위한 QuEChERS 분석법을 개발하고자 하였으며 그 결과를 QuEChERS AOAC Official 2007. 01법을 적용한 LC-MS/MS 분석결과와 비교하였다. QuEChERS AOAC Official 2007. 01법을 이용한 네가지 과일별 회수율은 각각 사과 71.1~104%, 포도 75.7~132.2%, 배 84.8~108.7%, 감 78.3~127.4%이었으며, 개선된 QuEChERS법을 이용한 네가지 작물별 회수율은 각각 사과 70.9~112.9%, 포도 71.3~101, 배 71.3~126%, 감 76.4~122.5% 이었으며, 두 방법 모두 다성분 분석법의 회수율 기준인 70~130%이내 조건을 만족하였다. 대부분의 농약이 변형한 방법으로 실험을 수행하였을 때 좋은 회수율이 보이므로 ECD, NPD 및 UVD와 같이 현재 분석기관에서 많이 보급된 분석 장비로 사용하여 다성분 동시분석이 가능할 것으로 판단되었다. 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.
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Tandem mass spectrometry has become a powerful tool for basic and applied mass spectrometry studies. Mass spectrometers based on ion trapping techniques, such as the quadrupole ion trap, have some unique capabilities as tandem mass spectrometers. Of particular note are the high MS–MS efficiency, the ability to perform multiple stages of tandem spectrometry (MSn), and the ability to effect ion–molecule reactions as part of the experimental sequence. This paper discusses the MSn experiment in a quadrupole ion trap and provides several examples of MSn experiments in which ion–molecule reactions are incorporated as one or more steps in the experiment. Examples include one in which MSn is used to determine the structure of an ion–molecule reaction product, one that involves multiple stages of collision-induced dissociation to generate a 13C containing reactant ion for an isotopic study, and one in which ion–molecule reactions are used to differentiate isomeric ion structures.
Top-down proteomics
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The determination of pesticide residues in oilseeds is a formidable challenge because compound pesticides are widely used in farming oilseeds. In this work, a novel method named Sin-QuEChERS (single-step, cheap, effective, rugged, safe) was established for the analysis of multiple pesticide residues in oil-bearing crop samples (rapeseed, peanut, sesame and melon seeds), based on the improvement of QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach. In the Sin-QuEChERS method, acetonitrile was used for sample extraction and primary-secondary amine (PSA) using C18 cartridge as purification media. By using Sin-QuEChERS, 38 pesticide residues in 4 oilseeds were detected by high performance liquid chromatography mass spectrometry (HPLC-MS/MS) within 5 min. and the correlation coefficient was more than 0.99. The average recoveries were 80.2 to 99.8%, and the relative standard deviation was less than 15%. Application of Sin-QuEChERS to monitor the pesticide residues of 100 batches of oilseeds showed that the established method was high throughput, accurate, sensitive, and reliable, and the limited detection ranged from 0.006 to 0.054 mg/kg.
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