Automated method development of sample preparation

Author(s):  
Chris Singleton ◽  
Ming Li
2019 ◽  
Vol 15 (7) ◽  
pp. 788-800 ◽  
Author(s):  
Natasa P. Kalogiouri ◽  
Victoria F. Samanidou

Background:The sample preparation is the most crucial step in the analytical method development. Taking this into account, it is easily understood why the domain of sample preparation prior to detection is rapidly developing. Following the modern trends towards the automation, miniaturization, simplification and minimization of organic solvents and sample volumes, green microextraction techniques witness rapid growth in the field of food quality and safety. In a globalized market, it is essential to face the consumers need and develop analytical methods that guarantee the quality of food products and beverages. The strive for the accurate determination of organic hazards in a famous and appreciated alcoholic beverage like wine has necessitated the development of microextraction techniques.Objective:The objective of this review is to summarize all the recent microextraction methodologies, including solid phase extraction (SPE), solid phase microextraction (SPME), liquid-phase microextraction (LPME), dispersive liquid-liquid microextraction (DLLME), stir bar sorptive extraction (SBSE), matrix solid-phase dispersion (MSPD), single-drop microextraction (SDME) and dispersive solid phase extraction (DSPE) that were developed for the determination of hazardous organic compounds (pesticides, mycotoxins, colorants, biogenic amines, off-flavors) in wine. The analytical performance of the techniques is evaluated and their advantages and limitations are discussed.Conclusion:An extensive investigation of these techniques remains vital through the development of novel strategies and the implication of new materials that could upgrade the selectivity for the extraction of target analytes.


2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
Bjoern B. Burckhardt ◽  
Stephanie Laeer

In USA and Europe, medicines agencies force the development of child-appropriate medications and intend to increase the availability of information on the pediatric use. This asks for bioanalytical methods which are able to deal with small sample volumes as the trial-related blood lost is very restricted in children. Broadly used HPLC-MS/MS, being able to cope with small volumes, is susceptible to matrix effects. The latter restrains the precise drug quantification through, for example, causing signal suppression. Sophisticated sample preparation and purification utilizing solid-phase extraction was applied to reduce and control matrix effects. A scale-up from vacuum manifold to positive pressure manifold was conducted to meet the demands of high-throughput within a clinical setting. Faced challenges, advances, and experiences in solid-phase extraction are exemplarily presented on the basis of the bioanalytical method development and validation of low-volume samples (50 μL serum). Enalapril, enalaprilat, and benazepril served as sample drugs. The applied sample preparation and extraction successfully reduced the absolute and relative matrix effect to comply with international guidelines. Recoveries ranged from 77 to 104% for enalapril and from 93 to 118% for enalaprilat. The bioanalytical method comprising sample extraction by solid-phase extraction was fully validated according to FDA and EMA bioanalytical guidelines and was used in a Phase I study in 24 volunteers.


Molecules ◽  
2020 ◽  
Vol 25 (22) ◽  
pp. 5297
Author(s):  
Kayla M. Billiard ◽  
Amanda R. Dershem ◽  
Emanuela Gionfriddo

Implementing green analytical methodologies has been one of the main objectives of the analytical chemistry community for the past two decades. Sample preparation and extraction procedures are two parts of analytical method development that can be best adapted to meet the principles of green analytical chemistry. The goal of transitioning to green analytical chemistry is to establish new methods that perform comparably—or superiorly—to traditional methods. The use of assessment tools to provide an objective and concise evaluation of the analytical methods’ adherence to the principles of green analytical chemistry is critical to achieving this goal. In this review, we describe various sample preparation and extraction methods that can be used to increase the greenness of a given analytical method. We gave special emphasis to modern microextraction technologies and their important contributions to the development of new green analytical methods. Several manuscripts in which the greenness of a solid-phase microextraction (SPME) technique was compared to other sample preparation strategies using the Green Analytical Procedure Index (GAPI), a green assessment tool, were reviewed.


2012 ◽  
Vol 95 (5) ◽  
pp. 1258-1271 ◽  
Author(s):  
José L Tadeo ◽  
Rosa Ana Pérez ◽  
Beatriz Albero ◽  
Ana I García-Valcárcel ◽  
Consuelo Sánchez-Brunete

Abstract This paper reviews the sample preparation techniques used for the analysis of pesticides in soil. The present status and recent advances made during the last 5 years in these methods are discussed. The analysis of pesticide residues in soil requires the extraction of analytes from this matrix, followed by a cleanup procedure, when necessary, prior to their instrumental determination. The optimization of sample preparation is a very important part of the method development that can reduce the analysis time, the amount of solvent, and the size of samples. This review considers all aspects of sample preparation, including extraction and cleanup. Classical extraction techniques, such as shaking, Soxhlet, and ultrasonic-assisted extraction, and modern techniques like pressurized liquid extraction, microwave-assisted extraction, solid-phase microextraction and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) are reviewed. The different cleanup strategies applied for the purification of soil extracts are also discussed. In addition, the application of these techniques to environmental studies is considered.


1979 ◽  
Vol 62 (3) ◽  
pp. 503-508 ◽  
Author(s):  
Larry L Wall ◽  
Charles W Gehrke

Abstract An automated urease-chromous colorimetric method (AUCM) has been developed for determining nitrogen in fertilizers. The method is applicable to fertilizer samples that contain only ammoniacal, nitrate, and urea nitrogen. The concept of this method, combining nitrate reduction and enzymatic urea hydrolysis to produce a single method for total nitrogen, is new. The AUCM is an almost totally automated method with only an acidic dissolution step as the manual sample preparation. The urea is hydrolyzed to ammonia and carbon dioxide with urease, and the nitrate is reduced to ammonia with chromous ion within the continuous flow analytical system. The final step, also within the analytical system, is the spectrophotometric measurement of the ammonia, employing the ammonia-salicylate-hypochlorite chemistry. The sampling rate is 30 samples/hr. The method is not applicable to fertilizer samples containing refractory organic nitrogen forms, water-insoluble nitrogen, or significant levels of biuret. The average per cent nitrogen recovery by the AUCM for ammonium nitrate-diammonium phosphate bulk-blended fertilizer samples was 99.7, suspensions and liquids 99.7, urea fertilizers 97.8, and urea-diammonium phosphate bulk blends 98. The relative standard deviation for the analytical system was 0.40%, and for the method, 0.70%. The sample preparation is short and simple. This method offers many advantages as a screening method for fertilizer industry and control laboratories.


2020 ◽  
Vol 12 (21) ◽  
pp. 9074 ◽  
Author(s):  
Daniela Thomas ◽  
Berit Schütze ◽  
Wiebke Mareile Heinze ◽  
Zacharias Steinmetz

Although most plastic pollution originates on land, current research largely remains focused on aquatic ecosystems. Studies pioneering terrestrial microplastic research have adapted analytical methods from aquatic research without acknowledging the complex nature of soil. Meanwhile, novel methods have been developed and further refined. However, methodical inconsistencies still challenge a comprehensive understanding of microplastic occurrence and fate in and on soil. This review aims to disentangle the variety of state-of-the-art sample preparation techniques for heterogeneous solid matrices to identify and discuss best-practice methods for soil-focused microplastic analyses. We show that soil sampling, homogenization, and aggregate dispersion are often neglected or incompletely documented. Microplastic preconcentration is typically performed by separating inorganic soil constituents with high-density salt solutions. Not yet standardized but currently most used separation setups involve overflowing beakers to retrieve supernatant plastics, although closed-design separation funnels probably reduce the risk of contamination. Fenton reagent may be particularly useful to digest soil organic matter if suspected to interfere with subsequent microplastic quantification. A promising new approach is extraction of target polymers with organic solvents. However, insufficiently characterized soils still impede an informed decision on optimal sample preparation. Further research and method development thus requires thorough validation and quality control with well-characterized matrices to enable robust routine analyses for terrestrial microplastics.


Author(s):  
Seema R. Nikam ◽  
Amol S. Jagdale ◽  
Sahebrao S. Boraste ◽  
Shrikant B Patil

Quantitatively measurements of chemical and biological drugs and their metabolites in the biological sample. This used in clinical and non-clinical studies. Non clinical including Pharmacokinetic and Toxic kinetic study, and clinical including Bioavailability, Bioequivalence study. This are play significant role and help in improvement in technology and analytical methods. Recent years have witnessed the introduction of several high- quality review articles into the literature covering various scientific and technical aspects of bioanalysis. Method validation and development use for the purpose of suitability of method for their intended purpose, this are important in Drug Discovery and Development. It including a validation parameters are Accuracy, Precision, Range, Calibration Curve, Recovery, Limit of Detection, Limit of Quantitation, Specificity, Selectivity and Stability, Ruggedness. This applicable in bio analysis, FDA and EMA guidelines. There are 3 main Extraction techniques used in sample preparation in bioanalysis is precipitation, liquid –liquid extraction, solid phase extraction. Detection of analyte by using hyphenated and chromatographic techniques like LC-MS/MS, HPLC, GC-MS. This LC-MS/MS is commonly used in a bioanalysis. This bio analysis study used in Pharmaceutical, Biomedical research purpose. Many challenges in pharmaceutical industry that fulfill by the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality.


2012 ◽  
Vol 84 (18) ◽  
pp. 7823-7830 ◽  
Author(s):  
Eva Tyteca ◽  
Anuschka Liekens ◽  
David Clicq ◽  
Ameriga Fanigliulo ◽  
Benjamin Debrus ◽  
...  

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