Fast sample preparation for analysis of tablets and capsules: the ball-mill extraction method

2001 ◽  
Vol 26 (4) ◽  
pp. 599-604 ◽  
Author(s):  
S.J. Kok ◽  
A.J.J. Debets
Nafta-Gaz ◽  
2021 ◽  
Vol 77 (5) ◽  
pp. 299-312
Author(s):  
Marek Janiga ◽  
◽  
Małgorzata Kania ◽  
Agnieszka Wciślak ◽  
Karol Spunda ◽  
...  

The aim of the work, the results of which are presented in the article, was to evaluate the influence of the method of sample preparation on the results of pyrolytic analyses: RockEval, Py-GC-FID (gas chromatography with FID detector) and Py-GC-IRMS (isotope mass spectrometry with gas chromatography). Mortars and ball mills are most often used to grind the samples. Three rock samples with a higher organic carbon content (shales) and five with a lower organic carbon content (including two samples of dolomites and three of anhydrites) were prepared. The rocks were homogenized and divided into three parts. Each part was ground: by hand in a mortar, in a ball mill for 5 minutes, and in a ball mill for 15 minutes. A total of 24 RockEval analyses, 48 Py-GC-FID analyses (two pyrolysis temperatures corresponding to RockEval pyrolysis conditions) and 24 Py-GC-IRMS analyses were performed. The grinding of the samples for the RockEval analyses is insignificant. The differences in the results seem to indicate the influence of the analysis error and the nature of the sample. For the Py-GC-FID methodology, the influence of milling on the results of desorption carried out at the temperature of 300ºC for most of the tested samples can be considered insignificant and negligible. At the temperature of 500ºC, various types of samples show some correlations, but they are insufficient to reject one of the methods of sample preparation. Therefore, it is important to analyze the results comprehensively, taking into account both the group composition and the distribution of pyrolysis products. In the case of the isotopic composition analyses (Py-GC-IRMS), also no differences in δ13C values related to different types of grinding samples can be found. Summarizing, all the results show a negligible influence of the method of grinding the samples on the results of pyrolysis analyses. Nevertheless, it is important that only one method of sample preparation is used for a separate sample series.


2015 ◽  
Vol 7 (4) ◽  
pp. 1509-1516 ◽  
Author(s):  
Fadi L. Alkhateeb ◽  
Kevin B. Thurbide

A novel micro pressurized liquid extraction (μPLE) method is introduced, which employs rapid heating in a static mode to remove analytes from 5–10 mg samples in as little as 10 seconds using only 125 μL of solvent.


Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4698
Author(s):  
Sorel Tchewonpi Sagu ◽  
Gerd Huschek ◽  
Thomas Homann ◽  
Harshadrai M. Rawel

The detection and quantification of nut allergens remains a major challenge. The liquid chroma-tography tandem mass spectrometry (LC-MS/MS) is emerging as one of the most widely used methods, but sample preparation prior to the analysis is still a key issue. The objective of this work was to establish optimized protocols for extraction, tryptic digestion and LC-MS analysis of almond, cashew, hazelnut, peanut, pistachio and walnut samples. Ammonium bicar-bonate/urea extraction (Ambi/urea), SDS buffer extraction (SDS), polyvinylpolypyrroli-done (PVPP) extraction, trichloroacetic acid/acetone extraction (TCA/acetone) and chloro-form/methanol/sodium chloride precipitation (CM/NaCl) as well as the performances of con-ventional tryptic digestion and microwave-assisted breakdown were investigated. Overall, the protein extraction yields ranged from 14.9 ± 0.5 (almond extract from CM/NaCl) to 76.5 ± 1.3% (hazelnut extract from Ambi/urea). Electrophoretic profiling showed that the SDS extraction method clearly presented a high amount of extracted proteins in the range of 0–15 kDa, 15–35 kDa, 35–70 kDa and 70–250 kDa compared to the other methods. The linearity of the LC-MS methods in the range of 0 to 0.4 µg equivalent defatted nut flour was assessed and recovery of internal standards GWGG and DPLNV(d8)LKPR ranged from 80 to 120%. The identified bi-omarkers peptides were used to relatively quantifier selected allergenic protein form the inves-tigated nut samples. Considering the overall results, it can be concluded that SDS buffer allows a better protein extraction from almond, peanut and walnut samples while PVPP buffer is more appropriate for cashew, pistachio and hazelnut samples. It was also found that conventional overnight digestion is indicated for cashew, pistachio and hazelnut samples, while microwave assisted tryptic digestion is recommended for almond, hazelnut and peanut extracts.


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