Rapid Sample Preparation Method Research Articles

Microwave-Assisted Method for Simultaneous Extraction and Hydrolysis for Determination of Flavonol Glycosides in Ginkgo Foliage Using Brönsted Acidic Ionic-Liquid [HO3S(CH2)4mim]HSO4 Aqueous Solutions

The Brönsted acidic ionic-liquid [HO3S(CH2)4mim] HSO4, a novel dual catalyst–solvent, has been successfully applied in simultaneous microwave-assisted extraction and hydrolysis for the determination of flavonol glycosides in Ginkgo foliage. The parameters, namely the [HO3S(CH2)4mim]HSO4 concentration, microwave-irradiation power, microwave-irradiation time, and solid–liquid ratio, were optimized. The optimum conditions were: an amount of 1.5 M [HO3S(CH2)4mim]HSO4, a microwave-irradiation power of 120 W, an irradiation time of 15 min, and a solid–liquid ratio of 1:30 g/mL. Compared with traditional methods the proposed approach demonstrates higher efficiency in a shorter operating time, and is an efficient, rapid, and simple sample preparation method.

Rapid and cost-effective baculovirus sample preparation method as a viable alternative to conventional preparation for quantitative real-time PCR

The increasing use of the baculovirus expression vector system (BEVS) has generated significant interest into techniques for quantifying baculovirus stocks. One method involves the use of quantitative real-time polymerase chain reaction (PCR). This study investigated simplifying baculovirus sample preparation for quantitative Real Time PCR to provide an alternative to current kit-based preparation methods. To achieve this goal, combinations of freeze/thaw cycles and Triton X-100 treatment were investigated. A treatment with only Triton X-100 was found to be sufficient to provide a simple, rapid and cheap alternative to kit-based preparation methods. This study also examined other factors such as primer choice to further examine the process of baculovirus quantitation by qPCR.

Determination of pesticide residues in milk using a QuEChERS-based method developed by response surface methodology

Response surface methodology (RSM) was employed to optimise a rapid and easy sample preparation method for the determination of 14 different pesticide residues in milk. The recovery of each pesticide was investigated by a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe)-based method with respect to 3 variables, the amounts of sodium acetate (Na Acetate), primary secondary amine (PSA), and octadecylsilane (C18). After optimisation, the maximum predicted recovery was the 99.73% rate for myclobutanil under the optimised conditions of 1.70g Na Acetate, 600.00mg PSA, and 489.96mg C18. The recovery rates of the other 9 hydrophilic pesticides were ranged from 82.01% to 98.84%. However, the recovery rates for the 4 lipophilic pesticides (2,4′-DDE, 4,4′-DDE, 2,4′-DDT, and 4,4′-DDT) were <80% because they were removed by C18 along with the other fatty compounds. This method could be implemented in many laboratories to reduce inspection time and cost.

Organic Solvent-Free and Simple Method for Determining Cyromazine and its Metabolite, Melamine, in Cow’s Milk

This paper described an organic solvent-free, rapid, simple, and space-saving method of sample preparation followed by HPLC coupled photo-diode array (PDA) detector for simultaneous quantification of cyromazine (CYR) and its decycropropylated metabolite, melamine (MEL), in milk. The HPLC-PDA was performed on an InertsilR HILIC column with an isocratic aqueous mobile phase. Analytes were extracted from the sample using water, and purified by MonoSpinR-C18, a centrifugal monolithic silica spin mini-columns, and quantified within 20 min. The method, performed under 100% aqueous conditions, obtained average recoveries for CYR and MEL in the range of 93.2 . 99.1% with relative standard deviations . 2.8%. The quantitation limits were 8.5 ng/mL for CYR and 10 ng/mL for MEL, respectively. No organic solvents were used at any stage of the analysis.

Organic Solvent-Free and Simple Method for Determining Cyromazine and Its Metabolite, Melamine, in Cow’s Milk

This paper described an organic solvent-free, rapid, simple, and space-saving method of sample preparation followed by HPLC coupled photo-diode array (PDA) detector for simultaneous quantification of cyromazine (CYR) and its decy-cropropylated metabolite, melamine (MEL), in milk. The HPLC-PDA was performed on an Inertsil? HILIC column with an isocratic aqueous mobile phase. Analytes were extracted from the sample using water, and purified by Mono-Spin?-C18, a centrifugal monolithic silica spin mini-columns, and quantified within 20 min. The method, performed under 100% aqueous conditions, obtained average recoveries for CYR and MEL in the range of 93.2% - 99.1% with relative standard deviations ≤ 2.8%. The quantitation limits were 8.5 ng/mL for CYR and 10 ng/mL for MEL, respectively. No organic solvents were used at any stage of the analysis.

Ultra-trace determination of plutonium in urine samples using a compact accelerator mass spectrometry system operating at 300 kV

Accelerator mass spectrometry (AMS) is a very sensitive and robust technique for analysis of long-lived radionuclides. Employment of the AMS technique can reduce the demands on sample preparation chemistry, due to its high rejection of interferences and low susceptibility to sample matrix. This is particularly of interest for ultra-trace determination of 239Pu in bioassay and environmental samples, as other mass spectrometric methods such as inductively coupled plasma mass spectrometry (ICP-MS) can suffer from isobaric mass interferences by the presence of uranium in the sample. A rapid sample preparation method for analysis of Pu at femtogram levels in large volume urine samples is described. Using the compact ETH AMS Tandy facility operating at ∼300 kV, the method was validated by analysing urine samples spiked with known amounts of 239/240/241Pu ranging from 1 to 30 fg. The detection limits for the method were estimated to be 0.38 fg for 239Pu, 0.40 fg for 240Pu and 0.08 fg for 241Pu in 1400 mL of urine.

Rapid Filtration Separation-Based Sample Preparation Method for Bacillus Spores in Powdery and Environmental Matrices

Authorities frequently need to analyze suspicious powders and other samples for biothreat agents in order to assess environmental safety. Numerous nucleic acid detection technologies have been developed to detect and identify biowarfare agents in a timely fashion. The extraction of microbial nucleic acids from a wide variety of powdery and environmental samples to obtain a quality level adequate for these technologies still remains a technical challenge. We aimed to develop a rapid and versatile method of separating bacteria from these samples and then extracting their microbial DNA. Bacillus atrophaeus subsp. globigii was used as a simulant of Bacillus anthracis. We studied the effects of a broad variety of powdery and environmental samples on PCR detection and the steps required to alleviate their interference. With a benchmark DNA extraction procedure, 17 of the 23 samples investigated interfered with bacterial lysis and/or PCR-based detection. Therefore, we developed the dual-filter method for applied recovery of microbial particles from environmental and powdery samples (DARE). The DARE procedure allows the separation of bacteria from contaminating matrices that interfere with PCR detection. This procedure required only 2 min, while the DNA extraction process lasted 7 min, for a total of <10 min. This sample preparation procedure allowed the recovery of cleaned bacterial spores and relieved detection interference caused by a wide variety of samples. Our procedure was easily completed in a laboratory facility and is amenable to field application and automation.

A mini‐electrodialysis system for desalting small volume saline samples for Fourier transform ion cyclotron resonance mass spectrometry

An affordable, commercially available mini‐electrodialysis (mini‐ED) system has been evaluated for the efficient desalting of small volume samples of seawater before analysis by electrospray Fourier transform ion cyclotron resonance mass spectrometry (ESI FT‐ICR MS). Mini‐ED FT‐ICR mass spectra were compared with spectra for samples that were treated by C18 solid phase extraction, a commonly used method for rapid sample preparation for this type of analysis. In this comparison, it is clear that mini‐ED provides more representative molecular information, compared with C18 isolation, and recovers the overwhelming majority of peaks from salt‐free samples, indicating that it adequately represents the DOM that can be ionized and analyzed by ESI FT‐ICR MS. The ED system produces a significant carbon blank. However, the substances contributing to this blank are not detectable by ESI FT‐ICR MS. Based on these findings mini‐ED is recommended as a promising method for the desalting of aqueous environmental samples before analysis by ESI FT‐ICR MS.

Determination of Trace Benzene Derivatives in Aqueous Samples by Ultrasonic Enhanced Hollow Fiber Liquid- Phase Microextraction Prior to Gas Chromatography

A new method was developed for the determination of trace compounds in water samples using ultrasonic-enhanced hollow fiber liquid-phase microextraction (U-HF-LPME). The ultrasonic radiation, which produces mechanical vibration and ultrasonic cavitation, could be used for accelerating the diffusion mass transfer process. Thus, ultrasonic was introduced into the HF-LPME procedure to enhance the mass-transfer rate during the aqueous and extraction solvent phases. Experimental parameters such as the extraction solvent, the extraction time, the ultrasonic frequency and power, the extractant volume, and ionic strength of the sample were assessed and optimized. Under optimal conditions, HF-LPME was achieved within 10 min. The high enrichment factor in the range of 120-666 and a good relative recovery in the range of 97-103% were evaluated with the relative standard deviations (RSDs, n = 5) of 0.3-7.0%. The limit of detection was in the range of 0.8-3.0 µg/L. The method was applied to the analysis of groundwater, lake water, and seawater. The results showed that the method can determine trace benzene derivatives in real samples with RSD values of 1.1-4.2%. The results demonstrated that U-HF- LPME is a rapid, accurate, and effective sample preparation method, and could be successfully applied for the determination of trace compounds in analytical chemistry.

Rapid separation and extraction of radioactive analytes onto filters and surfaces

Abstract This paper presents a radiochemical procedure that combines radiochemical sample preparation and analyte separation to provide a rapid sample preparation method. Extractive ligands are prepared in a polymer matrix. This system can be immobilized on a surface or on a filter. Filters allow rapid sample uptake due to the movement of the analyte through the filter material. These approaches offer fast uptake kinetics, high material loading, and good selectivity. These systems have been demonstrated for the rapid extraction of plutonium and americium from solution and their subsequent analysis by alpha spectrometry, with no additional sample preparation required, thus eliminating extensive wet chemical processes that would otherwise be necessary. We have evaluated the extraction efficiency that can be obtained and have shown that these systems can provide for alpha spectrometry peak widths near what can be obtained using traditional techniques such as electroplating. We have also demonstrated Polymer Ligand Films (PLFs) for the selective extraction of plutonium from a solution prepared from a soil digest.

RAPID DETERMINATION OF URANIUM ISOTOPES IN URINE BY INDUCTIVELY COUPLED PLASMA-MASS SPECTROMETRY

Following a radiological or nuclear emergency involving uranium exposure, rapid analytical methods are needed to analyze the concentration of uranium isotopes in human urine samples for early dose assessment. The inductively coupled plasma mass spectrometry (ICP-MS) technique, with its high sample throughput and high sensitivity, has advantages over alpha spectrometry for uranium urinalysis after minimum sample preparation. In this work, a rapid sample preparation method using an anion exchange chromatographic column was developed to separate uranium from the urine matrix. A high-resolution sector field ICP-MS instrument, coupled with a high sensitivity desolvation sample introduction inlet, was used to determine uranium isotopes in the samples. The method can analyze up to 24 urine samples in two hours with the limits of detection of 0.0014, 0.10, and 2.0 pg mL(-1) for (234)U, (235)U, and (238)U, respectively, which meet the requirement for isotopic analysis of uranium in a radiation emergency.

Automatic sample preparation of sulfonamide antibiotic residues in chicken breast muscle by using dynamic microwave-assisted extraction coupled with solid-phase extraction

In the work, a rapid, simple and high-throughput sample preparation method was developed for the determination of sulfonamide (SA) antibiotic residues in chicken breast muscle. The extraction and clean-up were online combined and up to 20 samples can be treated simultaneously in 6 min. The SAs were first extracted with acetonitrile under the action of microwave energy, and then the extract was directly introduced into the SPE column for on-line clean-up and concentration. Subsequently, the SAs eluted from the SPE column were determined by liquid chromatography-tandem mass spectrometry. The precisions of extraction results of 20 samples were in the range of 4.9-7.4%. The limits of detection and quantification obtained were in the range of 2.4-3.6 ng/g and 8.6-11.3 ng/g for SAs, respectively. The recoveries of SAs obtained by analyzing chicken muscles at three fortified levels (10, 50 and 500 ng/g) were in the range of 82.6-93.2%. The results of the validation process prove that the proposed method is suitable for treating numbers of complex samples simultaneously in a short time.

Discrimination of Alicyclobacillus Strains Using Nitrocellulose Membrane Filter and Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy

Alicyclobacillus spp. are thermoacidophilic, spore-forming bacteria, some of which cause spoilage in pasteurized and heat-treated apple juice products through the production of guaiacol. It would be helpful if a rapid method to detect and discriminate Alicyclobacillus strains was available. A simple and rapid sample preparation method using nitrocellulose membrane filter (NMF) and a single reflection horizontal attenuated total reflection (HATR) accessory with Fourier transform infrared (FT-IR) was developed here. Fourier transform infrared (FT-IR) spectroscopy was used and tested on 8 Alicyclobacillus strains (KF, WAC, NWN-13501, NWN-12697, NWN-12654, NWN-10682, 1016, 1101). A linear discriminant analysis (LDA) was established to discriminate Alicyclobacillus strains. The sample preparation method could successfully separated strains into different groups by principal component analysis (PCA). High identification accuracy (95%) was achieved with the LDA model. The method developed in the paper can be used to discriminate different Alicyclobacillus strains from each other making it possible to easily determine whether the strain of Alicyclobacillus present is associated with juice spoilage.

Rapid sample preparation for detection and identification of avian influenza virus from chicken faecal samples using magnetic bead microsystem

Avian influenza virus (AIV) is an infectious agent of birds and mammals. AIV is causing huge economic loss and can be a threat to human health. Reverse transcriptase polymerase chain reaction (RT-PCR) has been used as a method for the detection and identification of AIV virus. Although RT-PCR is a sensitive method for detection of AIV, it requires sample preparation including separation and purification of AIV and concentrate viral RNA. It is laborious and complex process especially for diagnosis using faecal sample. In this study, magnetic beads were used for immunoseparation of AIV in chicken faecal sample by a magnetic microsystem. Using this system, all the 16 hemagglutinin (H) and 9 neuraminidase (N) subtypes of AIV were separated and detected in spiked faecal samples using RT-PCR, without an RNA extraction step. This rapid sample preparation method can be integrated with a total analysis microsystem and used for diagnosis of AIV.

A simple and rapid method of sample preparation from culture filtrate of M. tuberculosis for two-dimensional gel electrophoresis

Sample preparation for Two-dimensional gel electrophoresis (2DE) is tedious and not sufficient to provide a comparative profile of secreted proteins for various strains of M. tuberculosis. High lipid content in mycobacteria limits the use of common methods as it can hinder the 2DE run. This study highlights the significance of SDS-TCA procedure over common used methods for the preparation of sample from culture filtrate as well as other proteinaceous fluids.

Simple and Rapid Determination of Organochlorine Pesticide Residues in Kampo Products by Gas Chromatography/Mass Spectrometry with Negative Chemical Ionization

A simple, rapid and inexpensive sample preparation method using extraction by shaking and sulfuric acid treatment was developed for determining eight organochlorine pesticides in kampo products by gas chromatography/mass spectrometry with negative chemical ionization. The recoveries were between 71% and 117%, and most relative standard deviations were less than 10%. The proposed method was applied to twenty-three samples of kampo formulae, and no samples were contaminated by eight organochlorine pesticides over the quantification limit.

Novel extraction method based on the dispersion of the extraction solvent for extraction of letrozole from biological fluids

The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. Dispersive liquid–liquid microextraction (DLLME) technique was successfully used as a simple, rapid and sensitive sample preparation method for the determination of letrozole in biological fluids and water samples. Chloroform at microlitre volume level and acetone were used as extraction and disperser solvents, respectively. The influence of several variables (e.g. type and volume of disperser and extraction solvents, ionic strength, etc.) on the performance of the sample preparation step was carefully evaluated. Under the optimum conditions, a preconcentration factor of 120 was obtained from only 10.0 mL of a water sample. The calibration graph was linear in the range of 1–500 μg L−1 with a detection limit of 0.3 μg L−1. The relative standard deviation (RSD) for five replicate measurements of letrozole was 3.2%. The calibration graphs were linear in the range of 2.5–500 μg L−1 and 5.0–500 μg L−1 with detection limits of 0.7 μg L−1 and 1.5 μg L−1 in urine and plasma samples, respectively. The relative recoveries of letrozole in plasma, urine and tap water samples at spiking levels of 50 μg L−1, 30 μg L−1 and 5 μg L−1 were 87.4%, 92.0% and 96.0%, respectively. DLLME combined with HPLC-UV is a fast, simple and efficient method for the determination of letrozole in biological fluids and water samples.

A rapid method of sample preparation for determining arsenic in water by stripping voltammetry

A procedure was developed for sample preparation for the further determination of arsenic in potable and natural water and process solutions by stripping voltammetry (SV). To minimize the losses and simplify the procedure, arsenic(III) was oxidized by the ozonation or UV irradiation of the solution in the presence of sulfite, chloride, or hydroxide ions, which increased the oxidation efficiency. The time required for 100% oxidation does not exceed 60 s for an arsenic concentration of no more than 1 mg/L. The reduction to arsenic(III) was performed photochemically in the presence of sodium sulfite for 5 min. Further stripping voltammetric determination was performed in the same solution using a gold-plated carbon electrode. The developed procedure is rapid, simple, and easy-to-automate.

Manual squeezing as an alternative to mechanical stomaching in preparing beef carcass sponge samples for microbiological analysis.

The U.S. Department of Agriculture (USDA) requires beef abattoir operators to periodically analyze beef carcass sponge samples for levels of Escherichia coli. Additional beef carcass sponge sampling is commonly used by processors to evaluate the efficacy of beef abattoir antimicrobial intervention systems. The USDA sample preparation procedure requires that beef carcass sponge samples be mechanically stomached for 2 min before the sample fluid is squeezed out for analysis. When a large number of sponge samples must be analyzed, the stomaching step can limit throughput. In this study, we compared the USDA sample preparation procedure with repeatedly squeezing the sponge during a 10-s interval to expel the sample fluid. Separate sponge samples were obtained from each half of 100 chilled postintervention beef carcasses from a large-volume abattoir during a 4-month period. The USDA and squeezing treatments were randomly assigned to the halves of each carcass. All sponge samples were analyzed for E. coli, coliforms, Enterobacteriaceae, and aerobic mesophilic bacteria using Petrifilm methods. The sample preparation method had no significant effect (signed rank value > 0.05) on the results of any analytical test, although aerobic mesophilic bacteria counts tended to be higher after the USDA method than after manual squeezing alone. These results suggest that manual squeezing may be a simple and rapid alternative sample preparation method when gram-negative bacteria such as E. coli, coliforms, or Enterobacteriaceae are being enumerated from beef carcass sponge samples used to monitor operational abattoir hygiene.

Simple and Rapid Determination of Cypermethrin and Fenvalerate Residues in Kampo Products by Gas Chromatography-Mass Spectrometry with Negative Chemical Ionization

In Japan, crude drugs that are used as ingredients of kampo formulae are mainly imported from China. In China, cypermethrin and fenvalerate, which are pyrethroid pesticides, are detected frequently in food exported to Japan. In fact, cypermethrin and fenvalerate have been detected in crude drugs distributed in Japan. There is concern that cypermethrin and fenvalerate will move from crude drugs to kampo products. Cypermethrin and fenvalerate in kampo products are controlled by a self-imposed residual pesticide limit set by the Japan Kampo Medicine Manufacturers Association. Several methods to analyze cypermethrin and fenvalerate in kampo products have been reported, but they are time-consuming, require expensive column clean-up, and use large amounts of organic solvents. In this study, a simple, rapid, and inexpensive sample preparation method was developed to determine cypermethrin and fenvalerate levels in kampo products by gas chromatography (GC)-mass spectrometry (MS) with negative chemical ionization (NCI). Twenty-two samples of kampo products were analyzed according to the proposed method. No samples were contaminated by cypermethrin and fenvalerate levels greater than the detection limit.