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1.
Bone Joint Res ; 6(9): 530-534, 2017 Sep.
Article in English | MEDLINE | ID: mdl-28899855

ABSTRACT

AIMS: The determination of the volumetric polyethylene wear on explanted material requires complicated equipment, which is not available in many research institutions. Our aim in this study was to present and validate a method that only requires a set of polyetheretherketone balls and a laboratory balance to determine wear. METHODS: The insert to be measured was placed on a balance, and a ball of the appropriate diameter was inserted. The cavity remaining between the ball and insert caused by wear was filled with contrast medium and the weight of the contrast medium was recorded. The volume was calculated from the known density of the liquid. The precision, inter- and intraobserver reliability, were determined by four investigators on four days using nine inserts with specified wear (0.094 ml to 1.626 ml), and the intra-class correlation coefficient was calculated. The feasibility of using this method in routine clinical practice and the time required for measurement were tested on 84 explanted inserts by one investigator. RESULTS: In order to get the mean for all investigators and determinations, the deviation between the measured and specified wear was -0.08 ml (sd 0.12; -0.21 to 0.11). The interobserver reliability was 0.989 ml (95% confidence interval (CI) 0.964 to 0.997) and the intraobserver reliability was 0.941 for observer 1 (95% CI 0.846 to 0.985), 0.983 for observer 2 (95% CI 0.956 to 0.995), 0.939 for observer 3 (95% CI 0.855 to 0.984), and 0.934 for observer 4 (95% CI 0.790 to 0.984). The mean time required to examine the samples was two minutes (sd 2; 1 to 5). CONCLUSION: The method presented here was shown to be sufficiently precise for many settings and is a cost-effective and quick method of determining the volumetric wear of explanted acetabular components. However, the measurement of wear for scientific purposes will probably continue to involve more accurate and dedicated laboratory equipment.Cite this article: Bone Joint Res 2017;6:530-534.

2.
Mini Rev Med Chem ; 3(6): 585-96, 2003 Sep.
Article in English | MEDLINE | ID: mdl-12871161

ABSTRACT

Since the discovery of E-64 in 1978 as potent cysteine protease inhibitor a variety of inhibitors containing small rings as electrophilic building blocks responsible for enzyme inhibition have been developed. In this review we summarize new aspects concerning epoxysuccinyl peptides derived from E-64 and discuss inhibition potency, selectivity and mechanisms of peptidic and peptidomimetic inhibitors containing epoxide, aziridine, thiirane, cyclopropane, beta-lactam and beta-lactone rings as electrophilic fragments.


Subject(s)
Cysteine Proteinase Inhibitors/chemistry , Cysteine Proteinase Inhibitors/pharmacology , Aziridines/chemistry , Aziridines/pharmacology , Cyclopropanes/chemistry , Cyclopropanes/pharmacology , Cysteine Endopeptidases/drug effects , Epoxy Compounds/chemistry , Epoxy Compounds/pharmacology , Humans , Lactams/chemistry , Lactams/pharmacology , Lactones/chemistry , Lactones/pharmacology , Structure-Activity Relationship , Sulfides/chemistry , Sulfides/pharmacology
3.
Electrophoresis ; 17(1): 110-9, 1996 Jan.
Article in English | MEDLINE | ID: mdl-8907527

ABSTRACT

The effect of buffer conditions -- varying in salt type, pH, and concentration -- on the separation of 8-aminonaphthalene-1,3,6-trisulfonic acid (ANTS)-labeled monosaccharides and complex-type carbohydrates was investigated. Different buffer systems for high and low electroosmotic flow conditions were chosen: a phosphate and a citrate background electrolyte, each at pH 2.5, a phosphate buffer, pH 9.0, and a borate buffer at pH 9.5. All buffer systems displayed differences in resolution and selectivity. Phosphate and borate buffer demonstrated the greatest selectivity changes for ANTS-labeled carbohydrates. While separation in the phosphate system relies mainly on differences in the charge-to-mass-ratio, additional selectivity can be achieved with borate complexation of glycoconjugates. The use of borate buffers improved monosaccharide separations whereas complex carbohydrates showed a loss in resolution. The citrate background electrolyte at low pH caused no significant changes in the separation performance. The pH 9.0 phosphate buffer showed a reversed migration order of the ANTS conjugates with a decreased resolution, compared to the pH 2.5 phosphate buffer, due to the strong electroosmotic flow generated under high pH conditions. An ovalbumin-derived oligosaccharide library demonstrates the significance of buffer selectivity for complex carbohydrate separations. The separation in the acidic phosphate and the alkaline borate buffer generates a different pattern and only the combination of both buffer systems allows an appropriate assessment of sample complexity.


Subject(s)
Carbohydrates/isolation & purification , Electrophoresis, Capillary , Monosaccharides/isolation & purification , Naphthalenes , Acids , Alkalies , Animals , Borates , Buffers , Carbohydrate Conformation , Carbohydrate Sequence , Databases, Factual , Molecular Sequence Data , Oligosaccharides/chemistry , Ovalbumin/chemistry , Phosphates
4.
J Chromatogr A ; 720(1-2): 353-76, 1996 Jan 12.
Article in English | MEDLINE | ID: mdl-8601201

ABSTRACT

This review focuses on recent developments in sensitive detection modes for carbohydrates after separation by capillary electrophoretic methods. To bring detection sensitivity for carbohydrates analysis in line with current methods in protein sequencing, concentration detection limits of 10(-6) molar or better are required. A discussion of mass detection limits and concentration detection limits is followed by an overview of detection modes for natural and labeled carbohydrates. Amperometric detection and UV and laser-induced fluorescence detection after reductive amination, in particular with 8-aminonaphthalene-1,3,6-trisulfonic acid (ANTS), are discussed in more detail. Finally, the paper outlines developments to be expected in the near future, focusing on the needs in glycobiology such as improved sensitivity and selectivity.


Subject(s)
Carbohydrates/analysis , Electrophoresis, Capillary , Carbohydrate Conformation , Carbohydrate Sequence , Electrophoresis, Capillary/instrumentation , Electrophoresis, Capillary/methods , Molecular Sequence Data , Spectrometry, Fluorescence , Spectrophotometry, Ultraviolet
5.
J Chromatogr A ; 716(1-2): 241-7, 1995 Nov 17.
Article in English | MEDLINE | ID: mdl-8574387

ABSTRACT

Complex oligosaccharides, both neutral and sialylated, were derivatized with 8-aminonaphthalene-1,3,6-trisulfonic acid (ANTS) and separated by capillary electrophoresis. The derivatization reaction was carried out in a total reaction volume of 2 microliters. The separated peaks were detected by laser-induced fluorescence detection using the 325-nm line of a He-Cd laser. Concentration and mass detection limits of 5 x 10(-8) M and 500 amol, respectively, could be achieved. The limiting step for higher sensitivity is not the detector performance, however, but the chemistry with a derivatization limit of 2.5 x 10(-6) M. Two labelling protocols were established, one with overnight reaction at 40 degrees C and the other with a 2.5-h derivatization time at 80 degrees C. Neutral oligosaccharides could be labelled with either protocol. However, sialylated oligosaccharides hydrolysed when labeled at 80 degrees C. Low nanomole to picomole amounts of oligomannose-type and complex-type oligosaccharide mixtures were derivatized and separated in less than 8 min with excellent resolution using a phosphate background electrolyte at pH 2.5. The linear relationship between the electrophoretic mobility and the charge-to-mass ratios of the ANTS conjugates was used for peak assignment. Further, the influence of the three-dimensional structure of the complex oligosaccharides on their migration behaviour is discussed. The suitability of the ANTS derivatization and the subsequent separation for the analysis of complex oligosaccharide patterns is demonstrated with oligosaccharide libraries derived from ovalbumin and bovine fetuin. For peak assignment the patterns are compared with those of the oligomannose and the complex-type oligosaccharide mixtures.(ABSTRACT TRUNCATED AT 250 WORDS)


Subject(s)
Oligosaccharides/isolation & purification , Animals , Cattle , Coloring Agents , Electrophoresis, Capillary , Lasers , Naphthalenes , Oligosaccharides/chemistry , Ovalbumin/chemistry , Sialic Acids/chemistry , Spectrometry, Fluorescence , alpha-Fetoproteins/analysis
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