THE EFFECT OF METHOD OF SAMPLE PREPARATION UPON THE DETERMINATION OF SOLUBILIZED INTRAMUSCULAR COLLAGEN FROM BOVINE MUSCLE BY QUANTITATION OF ITS HYDROXYPROLINE CONTENT

1980 ◽  
Vol 60 (3) ◽  
pp. 627-634 ◽  
Author(s):  
L. E. JEREMIAH ◽  
A. C. MURRAY ◽  
A. H. MARTIN
Keyword(s):  
Sample Preparation ◽  
Liquid Nitrogen ◽  
Muscle Tissue ◽  
Recovery Rate ◽  
Freeze Drying ◽  
Soluble Fraction ◽  
Collagen Content ◽  
Hydroxyproline Content ◽  
Bovine Muscle

A total of 91 muscle samples were utilized in a series of three separate but related experiments to evaluate possible effects of method of sample preparation upon the yields of intramuscular hydroxyproline from the heat-soluble, insoluble and combined fractions of bovine muscle tissue. The combined results of these experiments indicate that yields of intramuscular hydroxyproline, and thereby yields of intramuscular collagen, obtained in different studies can not be compared unless the same muscle is evaluated and the same method of sample preparation is employed in both and/or all studies in which yields are to be compared. Results from these experiments may also suggest that sample preparation, in which samples are frozen in liquid nitrogen, results in underestimation of intramuscular hydroxyproline content, and thereby intramuscular collagen content, from the heat-soluble fraction as evidenced by: (1) the substantially lower yields of intramuscular hydroxyproline from the heat-soluble fraction of samples frozen in liquid nitrogen; (2) the fact that added hydroxyproline was completely recovered in the heat-soluble fraction of muscle during preliminary experiments; and (3) the fact that method of sample preparation (freeze drying vs. direct homogenization) did not influence the recovery rate or result in overestimation of added hydroxyproline.

scholarly journals A Toolbox for the Determination of Nitroaromatic Explosives in Marine Water, Sediment, and Biota Samples on Femtogram Levels by GC-MS/MS

Toxics ◽  
2021 ◽  
Vol 9 (3) ◽  
pp. 60
Author(s):  
Tobias Hartwig Bünning ◽  
Jennifer Susanne Strehse ◽  
Ann Christin Hollmann ◽  
Tom Bötticher ◽  
Edmund Maser
Keyword(s):  
Sample Preparation ◽  
Freeze Drying ◽  
Solid Phase ◽  
Phase Extraction ◽  
Direct Extraction ◽  
Time Saving ◽  
Marine Samples ◽  
Volume Method ◽  
Biota Samples

To determine the amount of the explosives 1,3-dinitrobenzene, 2,4-dinitrotoluene, 2,4,6-trinitrotoluene, and its metabolites in marine samples, a toolbox of methods was developed to enhance sample preparation and analysis of various types of marine samples, such as water, sediment, and different kinds of biota. To achieve this, established methods were adapted, improved, and combined. As a result, if explosive concentrations in sediment or mussel samples are greater than 10 ng per g, direct extraction allows for time-saving sample preparation; if concentrations are below 10 ng per g, techniques such as freeze-drying, ultrasonic, and solid-phase extraction can help to detect even picogram amounts. Two different GC-MS/MS methods were developed to enable the detection of these explosives in femtogram per microliter. With a splitless injector, limits of detection (LODs) between 77 and 333 fg/µL could be achieved in only 6.25 min. With the 5 µL programmable temperature vaporization—large volume method (PTV-LVI), LODs between 8 and 47 fg/µL could be achieved in less than 7 min. The detection limits achieved by these methods are among the lowest published to date. Their reliability has been tested and confirmed by measuring large and diverse sample sets.

Freeze-drying enables homogeneous and stable sample preparation for determination of fecal short-chain fatty acids

2020 ◽  
Vol 589 ◽  
pp. 113508 ◽  
Author(s):  
Jun Ueyama ◽  
Masaya Oda ◽  
Masaaki Hirayama ◽  
Kuniyo Sugitate ◽  
Norihiro Sakui ◽  
...  
Keyword(s):  
Fatty Acids ◽  
Sample Preparation ◽  
Freeze Drying ◽  
Short Chain Fatty Acids ◽  
Short Chain ◽  
Chain Fatty Acids

scholarly journals DETERMINATION OF IODINE CONCENTRATION AND DISTRIBUTION IN RAT THYROID FOLLICLES BY ELECTRON-PROBE MICROANALYSIS

1969 ◽  
Vol 43 (1) ◽  
pp. 115-121 ◽  
Author(s):  
William L. Robison ◽  
David Davis
Keyword(s):  
Sample Preparation ◽  
Electron Probe Microanalysis ◽  
Electron Probe ◽  
Freeze Drying ◽  
Iodine Concentration ◽  
Sodium Concentration ◽  
Thyroid Glands ◽  
The Mean ◽  
Rat Thyroid

The concentration and the distribution of iodine in various sized follicles of rat thyroid glands have been analyzed by electron-probe microanalysis. The results of the iodine analysis were grouped according to uncorrected lumen diameter size. No significant differences in iodine concentration were observed among the various size categories. When the results for all follicles from a given sample were pooled, the standard error of the mean was approximately 4%. Usually 40–50 follicles per animal were analyzed. The concentration of iodine ranged from 0.9 to 2.1% by weight among individual animals. Scanning pictures and step-scan analysis showed the iodine distribution to be quite uniform across the colloid area. Several techniques of sample preparation were used; they produced no significant differences in the iodine concentrations observed. Sodium concentration, also determined in all samples, was found to vary from 2 to 9% by weight. Because of the mobility of the sodium ion, its distribution was greatly affected by the method of sample preparation. The technique that best preserved the natural chemistry of the sample was that of freezing the tissue, sectioning, and then freeze-drying.

Automated enzymatic determination of glycogen in bovine muscle tissue

1981 ◽  
Vol 172 (6) ◽  
pp. 454-456 ◽  
Author(s):  
Nel Haagsma ◽  
Klaas J. W. Kruithof ◽  
Betty G. M. Gortemaker
Keyword(s):  
Muscle Tissue ◽  
Bovine Muscle ◽  
Enzymatic Determination

scholarly journals Determination of Zeranol and its Metabolites in Bovine Muscle Tissue with Gas Chromatography-Mass Spectrometry

2012 ◽  
Vol 56 (3) ◽  
pp. 335-342 ◽  
Author(s):  
Iwona Matraszek-Żuchowska ◽  
Barbara Woźniak ◽  
Jan Żmudzki
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Muscle Tissue ◽  
Solid Phase ◽  
Performance Criteria ◽  
Gas Chromatography Mass Spectrometry ◽  
The European Union ◽  
Bovine Muscle ◽  
Chromatography Mass Spectrometry

Abstract This paper describes the quantitative method of determination of chosen substances from resorcylic acid lactones group: zeranol, taleranol, α-zearalenol, β-zearalenol, and zearalanone in bovine muscle tissue. The presented method is based on double diethyl ether liquid-liquid extraction (LLE), solid phase extraction (SPE) clean up, and gas chromatography mass spectrometry (GC-MS) analysis. The residues were derivatised with a mixture of N-methyl-N-trimethylsilyltrifluoroacetamide, ammonium iodide, and DL-dithiothreitol (1,000:2:5, v/w/w). The GC-MS apparatus was operated in positive electron ionisation mode. The method was validated according to the European Union performance criteria pointed in Decision Commission 2002/657/EC. The average recoveries of all analytes at 1 μg kg-1 level were located between 83.7% and 94.5% values with the coefficients of variation values <25%. The decision limits (CCα) and detection capabilities (CCβ) for all analytes ranged from 0.58 to 0.82 μg kg-1 and from 0.64 to 0.94 μg kg-1, respectively. The procedure has been accredited and is used as a screening and confirmatory method in control of hormone residues in animal tissues.

scholarly journals Multiresidue Liquid Chromatographic Method for Determining Residues of Mono- and Dibasic Penicillins in Bovine Muscle Tissues

1998 ◽  
Vol 81 (6) ◽  
pp. 1113-1120 ◽  
Author(s):  
Joe O Boison ◽  
Lily J -Y Keng
Keyword(s):  
Muscle Tissue ◽  
Phosphate Buffer ◽  
Chromatographic Method ◽  
Sodium Thiosulfate ◽  
Laboratory Method ◽  
Penicillin G ◽  
Bovine Muscle ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method with UV detection at 325 nm was developed for simultaneous determination of amoxicillin, ampicillin, penicillin G, and cloxacillin residues in bovine muscle tissue as their mercaptide derivatives. The penicillins are extracted from bovine tissues with 0.1 M phosphate buffer (pH 8.5), cleaned up on a t-C18 Sep-Pak cartridge, and eluted with 2 ml acetonitrile. After the acetonitrile in the eluate is evaporated to dryness, the residue is dissolved in 200 |µL (40 + 60, v/v) aceton itrile-phosphate buffer (pH 6.5) and derivatized with acetic anhydride and mercuric chloride in the presence of 1,2,4-triazole at 65°C for 30 min. Gradient analysis on a Spherisorb 5 µm ODS(2) (octadecyl silane) analytical column using a binary mobile phase consisting of acetonitrile and 0.10M phosphate buffer (pH 6.5) in the presence of 0.0157M sodium thiosulfate at 1 mL/min permits determination of each intact penicillin in bovine muscle tissue at ≥10 ppb with recoveries ≥72%. This laboratory method provides detection sensitivities equivalent to those of rapid tests used for screening β-lactam drug residues in bovine tissue samples for regulatory enforcement.

A cryo-SEM technique developed and applied to surfactant liposomes

1993 ◽  
Vol 51 ◽  
pp. 284-285
Author(s):  
Kiran Bhadriraju ◽  
Jayesh Bellare
Keyword(s):  
Sample Preparation ◽  
Liquid Nitrogen ◽  
Freeze Drying ◽  
Freezing Point ◽  
Freeze Fracture ◽  
Depth Of Field ◽  
Particle Sizes ◽  
Copper Sheet ◽  
Freeze Etching ◽  
Liquid Nitrogen Bath

Freeze-fracture replication TEM and Cryo-TEM are developed techniques for studying surfactant dispersions. Application of freeze-fracture cryo-SEM with direct imaging to such systems has the advantages of observing a greater range of particle sizes, large depth of field implying larger tilts together with rotation, and freeze-etching/freeze drying the sample while imaging it. A procedure for cryo-SEM of liquid colloids, which uses a simple sample preparation setup, and its results for liposomal dispersions, are described here.Samples are plunge-frozen by a freezing device (Fig.l) made from a standard desoldering tool (Fig.2) used as a plunging unit. Fracture plates (Fig.3) are made from 0.1 mm thin copper sheet made adhesive to the liquid by 400 mesh TEM grids that are bent over the two edges of the plates and stuck on the non-sample side with a rubber adhesive. The sample is sandwiched between a pair of fracture plates (Fig.3) and plunged into liquid Freon-22 kept at its freezing point (-160°C) in an electrically heated cup (Fig.l) cooled by a liquid liquid nitrogen bath.

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