Rapid Sample Preparation Method Research Articles

Development of a liquid-nitrogen-induced homogeneous liquid-liquid microextraction of Co(II) and Ni(II) from water and fruit juice samples followed by atomic absorption spectrometry detection.

In this study, a simple and rapid sample preparation method named liquid-nitrogen-induced homogeneous liquid-liquid microextraction has been developed for the extraction and pre-concentration of Co(II) and Ni(II) ions before their analysis by flame atomic absorption spectrometry. For this purpose, first, acetonitrile containing 8-hydroxyquinoline is added into a sample solution and the mixture is vortexed. As a result, a homogeneous solution is formed. Subsequently, the solution is cooled using liquid nitrogen for a few seconds. By this process, due to difference in the freezing point of acetonitrile and water, the homogeneous state is broken and the analytes (as oxinate complexes) are extracted into liquid acetonitrile phase collected on top of the frozen aqueous phase. The linear dynamic ranges obtained for Ni(II) and Co(II) were 1.0-30 and 0.50-20μgL-1, respectively. The obtained limits of detection were 0.36 and 0.20μgL-1 for Ni(II) and Co(II), respectively.

Development and validation of a GC-FID method for the analysis of short chain fatty acids in rat and human faeces and in fermentation fluids

Short-chain fatty acids (SCFAs) are gut microbiota metabolites recognized for their beneficial effects on the host organism. In this study, a simple and rapid sample preparation method combined to SCFAs analysis by direct injection and gas chromatography coupled with flame ionization detection (GC-FID), for the determination and quantification of eight SCFAs (acetic, propionic, i-butyric, butyric, i-valeric, valeric, i-caproic and caproic acids) in rat, mice and human faeces and in fermentation fluids samples, has been developed and validated. The method consists of extraction of the SCFAs by ethyl ether after acidification of the samples. The effect of the number of extractions has been assessed in order to optimize the procedure and to obtain a satisfactory yield for all the analyzed SCFAs. The increase of the extracted analytes quantity was significant passing from 1 to 2 and from 2 to 3 extractions (P < 0.05), while no significant differences were found performing 3, 4 or 5 extractions (P > 0.05). The SCFAs extracted are directly analyzed by GC-FID without derivatization and separated on a polyethylene glycol nitroterephthalic acid modified coated capillary column, with a chromatographic run time of 13 min. The proposed method showed good sensitivity, with limits of quantifications in the range 0.14–0.48 µM for SCFAs from propionic to caproic acids and 2.12 µM for acetic acid; recovery was between 80.8 and 108.8% and intraday and interday repeatability in the range 0.6–5.0% of precision (RSD, %) The optimized method is suitable for the quantitative analysis of SCFAs in real samples of rat, mouse and human faeces and in fermentation fluids, and it can be applied also to very small amount of faecal sample (20 mg).

Development of sample preparation method for organochlorine pesticides analysis in soil samples

OCPs are the persistent organic pollutants which are highly toxic to the environment and can accumulate in humans by foods such as rice, vegetable, and fruits. The aim of this research was to develop a rapid and easy sample preparation method for determination 4 OCPs, aldrin, dieldrin, β-endosulfane, and p-p' DDT in soil samples by gas chromatography with electron capture detection. The analysis was performed by using HP-5 capillary column with the isothermal condition at 250 oC and carrier gas flow rate of 1 mL/min. The results show that the 4 OCPs and internal standard, pentachloronitrobenzene, were analyzed within 6 min. The optimized condition of the sample preparation method was using ultrasonic assisted solvent extraction with 20 mL of hexane and ethyl acetate (9:1 v/v) as an extractant for 15x2 min. The results obtained from the proposed sample preparation method have demonstrated that the limit of detection was 0.628–3.68 μg kg-1. Percent recoveries were in the range of 81.42 to 110.7% and RSD were 1.68–9.43%. Correlation coefficients of calibration graphs were more than 0.99. The developed sample preparation method exhibited simplicity rapid and low chemical reagent consumption with satisfactory results.

Determination of Pyrethroids and Phthalate Esters in Radix et Rhizoma Glycyrrhizae by Successive Ultrasonic-assisted Extraction and Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

A rapid, inexpensive and efficient sample preparation method for simultaneous extraction and determination of three pyrethroids and seven phthalate esters in Radix et Rhizoma Glycyrrhizae samples was developed. The target analytes were extracted using a two-step extraction method including ultrasonic-assisted extraction and dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry (GC-MS). In ultrasonic-assisted extraction process, acetone was used as extraction solvent and extraction time was set as 3 min. In dispersive liquid-liquid microextraction process, optimized experimental conditions including 100 μL of CCl4 as extraction solvent and 1.0 mL of acetone as dispersant with 3% (m/V) of NaCl were adopted. The eluents were further quantitatively determined by GC-MS. All ten kinds of analytes were well separated, and the calibration curves showed good linearity, with correlation coefficients greater than 0.9992. Low detection limits of 0.0035 μg kg-1 for DMP to 1.0 μg kg-1 for IMIP were achieved. The method demonstrated good recoveries between the acceptable range of 79.7% for IMIP to 105.7% for TETR at three spiked levels with RSD < 8.2% for most of evaluated analytes. The method was employed for detection of Radix et Rhizoma Glycyrrhizae samples with satisfactory results.

Matrix-Induced Sugaring-Out: A Simple and Rapid Sample Preparation Method for the Determination of Neonicotinoid Pesticides in Honey.

In the present work, we developed a simple and rapid sample preparation method for the determination of neonicotinoid pesticides in honey based on the matrix-induced sugaring-out. Since there is a high concentration of sugars in the honey matrix, the honey samples were mixed directly with acetonitrile (ACN)-water mixture to trigger the phase separation. Analytes were extracted into the upper ACN phase without additional phase separation agents and injected into the HPLC system for the analysis. Parameters of this matrix-induced sugaring-out method were systematically investigated. The optimal protocol involves 2 g honey mixed with 4 mL ACN-water mixture (v/v, 60:40). In addition, this simple sample preparation method was compared with two other ACN-water-based homogenous liquid-liquid extraction methods, including salting-out assisted liquid-liquid extraction and subzero-temperature assisted liquid-liquid extraction. The present method was fully validated, the obtained limits of detection (LODs) and limits of quantification (LOQs) were from 21 to 27 and 70 to 90 μg/kg, respectively. Average recoveries at three spiked levels were in the range of 91.49% to 97.73%. Precision expressed as relative standard deviations (RSDs) in the inter-day and intra-day analysis were all lower than 5%. Finally, the developed method was applied for the analysis of eight honey samples, results showed that none of the target neonicotinoid residues were detected.

A rapid method of whole cell sample preparation for scanning electron microscopy using neodymium chloride

The quality of electron microscopy (EM) visualization of biological objects is constantly improving, primarily with the usage of more complex technologies, such as serial block-face scanning electron microscopy (SEM), focused ion beam scanning electron microscopy, and array tomography. Here we suggest a new rapid method of whole cell sample preparation for scanning EM using neodymium chloride treatment followed by staining with lead acetate. This variant of sample preparation does not require separate fixation, complete dehydration, and metal sputtering. By means of SEM in the back-scattered electron mode, in the neodymium-treated preparations, we visualized various morphological structures in human cells (nuclei with nucleoli, cytoskeleton, mitochondria) and microbial cells (Staphylococcus epidermidis, Streptococcus pneumoniae, Escherichia coli, and Candida albicans) preserving their species-specific shape and size. Thus, the suggested method provides additional information combining capabilities of SEM in visualizing cellular surface and transmission EM in detecting intracellular structures. Moreover, biological sample preparation with neodymium and lead is fast, informative, and cost-saving indicating a potential for its practical use for environmental SEM, and can be effectively combined with optical microscopy.

A novel two-dimensional liquid chromatography system for the simultaneous determination of three monoterpene indole alkaloids in biological matrices

The present paper describes a novel two-dimensional liquid chromatography (2D-LC) system, which is comprised of a first-dimensional ion exchange chromatography (IEX1) column, trap column, and second-dimensional reversed-phase chromatography (RP2) column system. The biological sample is separated by the first-dimensional LC using an IEX column to remove interferences. The analytes are transferred to the trap column after heart-cutting. Then, the analytes are transferred to the second-dimensional LC using an RP2 column for further separation and ultraviolet detection. This 2D-LC system can offer a large injection volume to provide sufficient sensitivity and exhibits a strong capacity for removing interferences. Here, the determination of three monoterpene indole alkaloids (MIAs; gelsemine, koumine, and humantenmine) from Gelsemium in biological matrices (plasma, tissue, and urine) was used this 2D-LC system. After a rapid and easy sample preparation method based on protein precipitation, the sample was injected into the 2D-LC. The method was developed and validated in terms of the selectivity, LOD, LOQ, linearity, precision, accuracy, and stability. The sample preparation time for the three MIAs was 15min. The LOD for these compounds was 10ng/mL, which was lower than the developed HPLC methods. The results showed that this method had good quantitation performance and allowed the determination of gelsemine, koumine, and humantenmine in biological matrices. The method is rapid, exhibits high selectivity, has good sensitivity, and is low-cost, thus making it well-suited for application in the pharmaceutical and toxicological analysis of Gelsemium. Graphical abstract.

Analyzing 2-acetyl-4(5)-(1,2,3,4-tetrahydroxybutyl)-imidazole in beverages by dispersive micro-solid phase extraction using polymer cation exchange sorbent followed by ion chromatography and liquid chromatography coupled with tandem mass spectrometry

The presence of 2-acetyl-4(5)-(1,2,3,4-tetrahydroxybutyl)-imidazole (THI) in beverages has raised several concerns regarding its toxicity to humans. The sample preparation and detection of THI in complex matrices is challenging owing to its high water solubility. Here we reported a rapid sample preparation method based on dispersive micro-solid phase extraction (D-μ-SPE) using polymer cation exchange sorbent as sorbent for the extraction of THI from beverage samples. THI was detected by high performance anion exchange chromatography-pulsed amperometric detector (HPAEC-PAD) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The experimental parameters of D-μ-SPE on extraction efficiency were carefully optimized. Under the optimized conditions, high recoveries (83.4–96.1%) and good reproducibility (%RSD ≤ 8.7%) were obtained using D-μ-SPE-HPAEC-PAD and D-μ-SPE-HPLC-MS/MS. Limit of quantification was 75 ng/mL for HPAEC-PAD and 5 ng/mL for HPLC-MS/MS. This work proves the potential application the newly developed method for the quantification of THI in beverages containing caramel color.

Performance of MALDI-TOF MS for the identification of gram-negative bacteria grown on eosin methylene blue (EMB) agar: A simple method for improving the effectiveness of identification

Matrix Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry (MALDI-TOF MS) is a new method that is increasingly used in microbiology laboratories due to its ability of reliable and rapid identification (ID) of bacteria and fungi. However, some problems emerge in the routine clinical diagnosis since only one gram-negative selective medium has been suggested up to date. Though EMB agar is one of the traditional gram-negative selective media, there is no data in the scientific literature, about the ID performance of MALDI TOF MS with the gram-negative bacteria grown on this medium. In this study, we tested the ID performance of MALDI-TOF MS for gram-negative isolates on EMB agar and aimed to develop a rapid and easy sample preparation method for improving this performance. A total of 468 clinical isolates of gram-negative bacteria, consisting of 37 different species from 20 genera, were included in this study. The isolates were identified using the Vitek MS MALDI-TOF MS (Bio Mérieux, France) both directly from EMB agar, and also through a two-step colony washing (once with physiologic saline, and three times with 70% ethanol) method. The performances of these two IDs were compared. In the direct reading from EMB medium, 382 (81.6%) of 468 studied isolates were correctly identified at species level; no ID was detected for 80 (17%) isolates, and 6 (1.2%) isolates (four at the genus level) were misidentified Performance of MALDI-TOF MS directly from EMB agar was excellent (100%) for 14 species including Stenotrophomonas maltophilia, Klebsiella oxytoca, Salmonella spp., and Proteus mirabilis; and lowest for Providencia spp. (62.5%), Escherichia coli (70.5%) and Acinetobacter spp. (70.7%). Following the washing procedure which was performed about 20 min with simple laboratory equipment, 434 (92.7%) isolates were correctly identified at species level; 30 (6.4%) strains could not be identified, and four (0.85%) isolates (two at the genus level) were misidentified. Statistical analyses indicated that the washing procedure defined here significantly increased the overall ID performance of MALDI-TOF MS with EMB agar (p= 0.001), particularly with improving the IDs of those markedly dye-absorbing genera, such as E.coli and A.baumannii. In this study, EMB agar which has no data until today on its suitability for mass spectrometric identification has been shown to be useful for bacterial identification with MALDI-TOF MS. In addition, the unidentified gram-negative bacteria in the direct reading from the EMB medium have been shown to be identified after the colony washing method as described here. Determination of the different medium alternatives will contribute to effective usage of MALDI-TOF MS in microbiology laboratories.

Salting-out-assisted liquid–liquid extraction of 5-hydroxymethylfurfural from honey and the determination of 5-hydroxymethylfurfural by high-performance liquid chromatography

A simple, rapid, and effective sample preparation method was developed for the recovery of 5-hydroxymethylfurfural from honey samples with negligible co-extracted sugars.

Phytoplasma detection and quantification: Make it easy

When high numbers of analyses are required a rapid sample preparation method coupled to RT-qPCR allows to reduce the time and the costs for the phytoplasma detection in plant samples. A comparison between DNA and RNA contribution to qPCR detection revealed the higher input of the latter ensuring the maintenance of the sensitivity and specificity of the assay. The protocol has been validated for the detection and quantification of ‘Candidatus Phytoplasma mali’, ‘Ca. P. pyri’, ‘Ca. P. prunorum’, ‘Ca. P. solani’ and “flavescence doree” phytoplasma by qPCR, RT-qPCR, ddPCR and ddRT-PCR techniques based on TaqMan chemistry.

MALDI-TOF MS Affords Discrimination of Deinococcus aquaticus Isolates Obtained From Diverse Biofilm Habitats.

Matrix-assisted Laser Desorption Ionization-Time of Flight Mass Spectroscopy (MALDI-TOF MS) has been used routinely over the past decade in clinical microbiology laboratories to rapidly characterize diverse microorganisms of medical importance both at the genus and species levels. Currently, there is keen interest in applying MALDI-TOF MS at taxonomic levels beyond species and to characterize environmental isolates. We constructed a model system consisting of 19 isolates of Deinococcus aquaticus obtained from biofilm communities indigenous to diverse substrates (concrete, leaf tissue, metal, and wood) in the Fox River – Lake Winnebago system of Wisconsin to: (1) develop rapid sample preparation methods that produce high quality, reproducible MALDI-TOF spectra and (2) compare the performance of MALDI-TOF MS-based profiling to common DNA-based approaches including 16S rRNA sequencing and genomic diversity by BOX-A1R fingerprinting. Our results suggest that MALDI-TOF MS can be used to rapidly and reproducibly characterize environmental isolates of D. aquaticus at the subpopulation level. MALDI-TOF MS provided higher taxonomic resolution than either 16S rRNA gene sequence analysis or BOX-A1R fingerprinting. Spectra contained features that appeared to permit characterization of isolates into two co-occurring subpopulations. However, reliable strain-level performance required rigorous and systematic standardization of culture conditions and sample preparation. Our work suggests that MALDI-TOF MS offers promise as a rapid, reproducible, and high-resolution approach to characterize environmental isolates of members of the genus Deinococcus. Future work will focus upon application of methods described here to additional members of this ecologically diverse and ubiquitous genus.

Quantification of eight active ingredients in crude and processed radix polygoni multiflori applying miniaturized matrix solid-phase dispersion microextraction followed by UHPLC.

A rapid, efficient, and green sample preparation method has been developed to extract eight active ingredients (gallic acid, catechins, epicatechin, polydatin, 2,3,5,4'-tetrahydroxystilbene-2-O-β-d-glucoside, resveratrol, emodin, and physcion) in radix polygoni multiflori by miniaturized matrix solid-phase dispersion microextraction. Simple and sensitive ultra high performance liquid chromatography combined with ultraviolet detection has been applied to analyze the multiple compounds. The best results were obtained by adding 25mg sample into 25mg adsorbent and grinding for 2min with disorganized silica as adsorbent and 1mL 150mM 1-dodecyl-3-methylimidazolium bromide as a green eluting solvent. Good linearity (r2 >0.998) for each analyte was obtained by this method. The intra-day and inter-day precision (RSD) were both below 5.31%, and the recoveries of the analytes ranged from 93.3 to 100.0%. This simple miniaturized matrix solid-phase dispersion microextraction method for analyzing the compounds in radix polygoni multiflori needs a short time and requires little sample and reagent. Thus, this method is far more eco-friendly and efficient than traditional extraction methods (reflux and ultrasound-assisted extraction). The present investigation provided a promising method for the fast preparation and discrimination of chemical differences in crude and processed radix polygoni multiflori.

A sublimate sorbent for stir-bar sorptive extraction of aqueous endocrine disruptor pesticides for gas chromatography-electron capture detection

A dumbbell-shaped magnetic stir-bar with sublimate sorbent was prepared for the stir bar sorptive extraction (SBSE) of pesticides in an aqueous sample prior to gas chromatography-micro-electron capture detection (GC-μECD). Cyclododecane (CDD) was coated onto a magnetic stir-bar surface as a sublimate sorbent, and steel balls were placed on both ends to form a dumbbell-shaped magnetic stir-bar for SBSE. Four EDC pesticides including chlorpyrifos, ethion, bromopropylate, and λ-cyhalothrin in aqueous samples were selected as model species to examine the proposed SBSE and the following desorption.The parameters studied were those affecting the extraction efficiencies including the coating (solvent for CDD and thickness), extraction (sample pH, stirring rate, time, and salting out effect), dissolution solvent volume, and the loss of CDD sublimated in air. The maximum extraction efficiency was obtained under the following conditions. The stir bar (with CDD thickness of 5.2 μm) was added into a 10 mL sample solution (at pH 7) for a 20-min extraction at 600 rpm. Then, the stir bar was gently removed from the sample solution, disassembled, and immersed into a 0.2 mL insert tube consisting of 3 μL hexane to dissolve; 1 μL was used for GC-ECD analysis. The linear ranges were 0.005–5 μg L−1 with coefficients of determination ranging from 0.9950 - 0.9994. Detection limits (based on S/N = 3) of the four EDCs were 0.4–4.5 ngL-1 with a relative standard deviation (RSD) of 2.4–6.3%, and quantitation limits (based on S/N = 5) were 1–15 ngL−1. The relative recoveries of the spiked samples were in the range of 83.2–98.7% with RSDs of 2.1–8.4% in farm field waters. The proposed sublimation sorbent obtained excellent enrichment factors (101–834) and provided a simple, rapid, sensitive, and eco-friendly sample preparation method.

Rapid Sample Preparation Method with High Lipid Removal Efficiency for Determination of Sulphuric Acid Stable Organic Compounds in Fish Samples

A rapid and low-cost sample preparation method modifying the so-called QuEChERS (quick, easy, cheap, effective, rugged and safe) method was developed for the determination of H2SO4 stable organic compounds in fish samples. The method involves acetonitrile salting-out extraction and a novel clean-up procedure combining the pH-tuned dispersive liquid–liquid microextraction (DLLME) with conc. H2SO4 digestion. The H2SO4 treatment is carried out by a simple operation in contrast to laborious and time-consuming procedures reported in the literature. The method was developed, optimised and validated using selected polybrominated diphenyl ethers (PBDEs) as representatives of H2SO4 stable compounds. For instrumental analysis of sample extracts, thermal desorption–gas chromatography–triple quadrupole tandem mass spectrometry (TD–GC–QqQ-MS/MS) was used. The proposed sample preparation method provides better co-extractives removal efficiency as compared to the original QuEChERS method and, unlike the QuEChERS dispersive solid-phase extraction (dSPE), allows complete removal of fatty acids. The sample preparation is low-cost due to the employment of small amounts of low-cost chemicals (no need of expensive sorbents), and it does not require special instrumentation. The whole analytical method showed satisfactory performance (linearity, recovery, repeatability, accuracy, limits of the method), and its applicability was confirmed by determination of PBDEs in samples of four fish species with variable lipid content in the range of 0.7–19%. The obtained recoveries for six PBDEs in the NIST standard reference material SRM 1946 were in the range of 81–95%, and relative standard deviations were in the range of 3–13%.

Portable platform for rapid in-field identification of human fecal pollution in water.

Human fecal contamination of water is a public health risk. However, inadequate testing solutions frustrate timely, actionable monitoring. Bacterial culture-based methods are simple but typically cannot distinguish fecal host source. PCR assays can identify host sources but require expertise and infrastructure. To bridge this gap we have developed a field-ready nucleic acid diagnostic platform and rapid sample preparation methods that enable on-site identification of human fecal contamination within 80 min of sampling. Our platform relies on loop-mediated isothermal amplification (LAMP) of human-associated Bacteroides HF183 genetic markers from crude samples. Oligonucleotide strand exchange (OSD) probes reduce false positives by sequence specifically transducing LAMP amplicons into visible fluorescence that can be photographed by unmodified smartphones. Our assay can detect as few as 17 copies/ml of human-associated HF183 targets in sewage-contaminated water without cross-reaction with canine or feline feces. It performs robustly with a variety of environmental water sources and with raw sewage. We have also developed lyophilized assays and inexpensive 3D-printed devices to minimize cost and facilitate field application.

Simultaneous determination of simazine, cyanazine, and atrazine in honey samples by dispersive liquid-liquid microextraction combined with high-performance liquid chromatography.

A rapid and simple sample preparation method was developed for simultaneous determination of three triazine herbicides in honey samples. The selected herbicides were extracted from honey samples by ionic liquid dispersive liquid-liquid microextraction, separated on a C18 column (250mm × 4.6mm id, 5μm) using acetonitrile and H2 O as the mobile phase with gradient elution, and then detected by high-performance liquid chromatography. The parameters, such as the type and volume of the extraction and disperser solvent, ion strength, pH, extraction time, and centrifuge time were optimized in order to provide the excellent extraction performance. Good linearity was showed for all the target herbicides over the tested concentration range with correlation coefficient higher than 0.994. Three spiked levels (0.005, 0.05, 0.10mg/kg) were applied for determination of the recoveries of the targets in honey samples in the range of 80-103% with relative standard deviations not larger than 10.6%. The limits of quantification for the analytes ranged between 1.5 and 4.0μg/kg. The developed method was applied for determination of the target compounds residues in real samples.

Deep eutectic solvent-based ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the determination of ultraviolet filters in water samples

In the present study, a simple and rapid sample preparation method designated ultrasound-assisted dispersive liquid-liquid microextraction based on a deep eutectic solvent (DES) followed by high-performance liquid chromatography with ultraviolet (UV) detection (HPLC-UVD) was developed for the extraction and determination of UV filters from water samples. The model analytes were 2,4-dihydroxybenzophenone (BP-1), benzophenone (BP) and 2-hydroxy-4-methoxybenzophenone (BP-3). The hydrophobic DES was prepared by mixing trioctylmethylammonium chloride (TAC) and decanoic acid (DecA). Various influencing factors (selection of the extractant, amount of DES, ultrasound duration, salt addition, sample volume, sample pH, centrifuge rate and duration) on UV filter recovery were systematically investigated. Under optimal conditions, the proposed method provided good recoveries in the range of 90.2–103.5% and relative standard deviations (inter-day and intra-day precision, n=5) below 5.9%. The enrichment factors for the analytes ranged from 67 to 76. The limits of detection varied from 0.15 to 0.30ngmL−1, depending on the analytes. The linearities were between 0.5 and 500ngmL−1 for BP-1 and BP and between 1 and 500ngmL−1 for BP-3, with coefficients of determination greater than 0.99. Finally, the proposed method was applied to the determination of UV filters in swimming pool and river water samples, and acceptable relative recoveries ranging from 82.1 to 106.5% were obtained.

Sample Preparation for Bioanalytical and Pharmaceutical Analysis.

Biological and pharmaceutical samples represent formidable challenges in sample preparation that hold important consequences for bioanalysis and genotoxic impurity quantification. This Feature will emphasize significant advances toward the development of rapid, sensitive, and selective sample preparation methods.

Solid-phase extraction combined with dispersive liquid-liquid microextraction for the determination of pyrethroid pesticides in wheat and maize samples.

A rapid, selective and sensitive sample preparation method based on solid-phase extraction combined with the dispersive liquid-liquid microextration was developed for the determination of pyrethroid pesticides in wheat and maize samples. Initially, the samples were extracted with acetonitrile and water solution followed phase separation with the salt addition. The following sample preparation involves a solid-phase extraction and dispersive liquid-liquid microextraction step, which effectively provide cleanup and enrichment effects. The main experimental factors affecting the performance both of solid-phase extraction and dispersive liquid-liquid microextration were investigated. The validation results indicated the suitability of the proposed method for routine analyze of pyrethroid pesticides in wheat and maize samples. The fortified recoveries at three levels ranged between 76.4 and 109.8% with relative standard deviations of less than 10.7%. The limit of quantification of the proposed method was below 0.0125 mg/kg for the pyrethoroid pesticides. The proposed method was successfully used for the rapid determination of pyrethroid residues in real wheat and maize samples from crop field in Beijing, China.