New Sampling/Sample Preparation Strategies for Rapid Screening

2002 ◽  
pp. 3-7
Author(s):  
J. Pawliszyn
1983 ◽  
Vol 66 (4) ◽  
pp. 825-849 ◽  
Author(s):  
Douglas I Mcgregor ◽  
William J Mullin ◽  
Gruffydd R Fenwick

Abstract New analytical techniques and instrumentation and increased knowledge of the diversity and distribution of glucosinolates, the diversity of their enzymatically released products, and factors influencing their release, have led to significant advances in methodology for analysis of glucosinolates over the past three decades. However, many of the methods have been developed for specific agricultural crops or commodities and their particular glucosinolate compositions. They can only be applied to certain types of plant material or can detect and quantitate only certain glucosinolates or their products. Other methods have been designed to meet specific research, regulatory, or quality control requirements. This had necessitated sacrifice of either speed, simplicity, accuracy, precision, or the ability to distinguish different glucosinolates or their products. This review examines the methods available for sample preparation, identification, and quantitation of glucosinolates in light of current knowledge of their diversity, distribution, and chemistry. Consideration is given to the suitability of methods for rapid screening or precise, discriminating measurement, and to the standardization of methodology and reporting of results.


2021 ◽  
Vol 3 ◽  
pp. e8
Author(s):  
Yao Gao ◽  
Tianwen Zhang ◽  
Shirong Huang ◽  
Xinxin Lin ◽  
Sisi Gong ◽  
...  

A precise analytical method was established for rapid screening of 49 antibiotic residues in aquatic products by ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-QToFMS). The quick, easy, cheap, effective, rugged and safe (QuEChERS) process was refined for effective sample preparation. The homogenized samples of aquatic products were extracted with 3% acetic acid in acetonitrile, salted out with anhydrous magnesium sulfate and sodium chloride, and cleaned up by octadecylsilane (C18) and primary-secondary amine (PSA) powder. Then, the purified samples were separated on a BEH C18 column using 0.1% formic acid and methanol as mobile phases by gradient elution, detected by MS under positive Electron Spray Ionization (ESI+) mode. The linear range of matrix-matched calibration curve was 1–100 μg/L for each compound with the correlation coefficients in the range of 0.9851–0.9999. The recoveries of target antibiotics at the different spiked levels ranged from 60.2% to 117.9% except for lincomycin hydrochloride, whereas relative standard deviations (RSDs) were between 1.6% and 14.0% except for sulfaguanidine in grass Carp, Penaeus vannamei and Scylla serrata matrices. The limits of detection (LODs) (S/N = 3) for the analytes were 0.05–2.40 μg/kg, 0.08–2.00 μg/kg and 0.10–2.27 μg/kg and the limits of quantification (LOQs) (S/N = 10) were 0.16–8.00 μg/kg, 0.25–6.66 μg/kg and 0.32–7.56 μg/kg in grass Carp, Penaeus vannamei and Scylla serrata, respectively. The method was successfully applied to grass Carp, Penaeus vannamei and Scylla serrata, demonstrating its ability for the determination of multi-categories antibiotic residues in aquatic products.


2020 ◽  
Vol 25 (4) ◽  
pp. 380-387 ◽  
Author(s):  
Ximo Zhang ◽  
Corey E. Reed ◽  
Robert E. Birdsall ◽  
Ying Qing Yu ◽  
Weibin Chen

Protein glycosylation can impact the efficacy and safety of biotherapeutics and therefore needs to be well characterized and monitored throughout the drug product life cycle. Glycosylation is commonly assessed by fluorescent labeling of released glycans, which provides comprehensive information of the glycoprofile but can be resource-intensive regarding sample preparation, data acquisition, and data analysis. In this work, we evaluate a comprehensive solution from sample preparation to data reporting using a liquid chromatography–mass spectrometry (LC-MS)-based analytical platform for increased productivity in released glycan analysis. To minimize user intervention and improve assay robustness, a robotic liquid handling platform was used to automate the release and labeling of N-glycans within 2 h. To further increase the throughput, a 5 min method was developed on a liquid chromatography–fluorescence–mass spectrometry (LC-FLR-MS) system using an integrated glycan library based on retention time and accurate mass. The optimized method was then applied to 48 released glycan samples derived from six batches of infliximab to mimic comparability testing encountered in the development of biopharmaceuticals. Consistent relative abundance of critical species such as high mannose and sialylated glycans was obtained for samples within the same batch (mean percent relative standard deviation [RSD] = 5.3%) with data being acquired, processed, and reported in an automated manner. The data acquisition and analysis of the 48 samples were completed within 6 h, which represents a 90% improvement in throughput compared with conventional LC-FLR-based methods. Together, this workflow facilitates the rapid screening of glycans, which can be deployed at various stages of drug development such as process optimization, bioreactor monitoring, and clone selections, where high-throughput and improved productivity are particularly desired.


2011 ◽  
Vol 28 (10) ◽  
pp. 1383-1392 ◽  
Author(s):  
Y. Shi ◽  
J.S. Chang ◽  
C.L. Esposito ◽  
C. Lafontaine ◽  
M.J. Berube ◽  
...  

Author(s):  
R. E. Ferrell ◽  
G. G. Paulson ◽  
C. W. Walker

Selected area electron diffraction (SAD) has been used successfully to determine crystal structures, identify traces of minerals in rocks, and characterize the phases formed during thermal treatment of micron-sized particles. There is an increased interest in the method because it has the potential capability of identifying micron-sized pollutants in air and water samples. This paper is a short review of the theory behind SAD and a discussion of the sample preparation employed for the analysis of multiple component environmental samples.


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