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81.
Enantiomeric purity determination of acetyl-l-carnitine by NMR with chiral lanthanide shift reagents
Miyuki Kagawa Yoshio Machida Hiroyuki Nishi Jun Haginaka 《Journal of pharmaceutical and biomedical analysis》2005,38(5):918
Enantiomer signal separation of acetyl-carnitine chloride was obtained on a 500 MHz Nuclear Magnetic Resonance (1H NMR) analysis by fast diastereomeric interaction with chiral shift reagents such as chiral lanthanide-camphorato or chiral samarium-pdta shift reagents. Effects of the kinds of chiral shift reagents and the molar ratio of chiral shift reagent to acetyl-carnitine chloride on enantiomer signal separation were investigated and evaluated. Optimization of the experimental conditions provided two significant split signals for the enantiomers, leading to the successful quantitative analysis. Distinguishment of 0.5% of the minor enantiomer (d-form) in acetyl-l-carnitine chloride was found to be possible by 1H NMR with tris[3-(heptafluoropropylhydroxymethylene)-d-camphorato] and praseodymium derivative, (Pr[hfc]3), as chiral shift reagents. 相似文献
82.
The recombinant 3C-like protease of Chiba virus, a Norovirus, expressed in Escherichia coli cells was purified and characterized as to effects of pH, temperature, salt contents, and SH reagents on its proteolytic activity. The optimal pH and temperature of the 3C-like protease for the proteolytic activity were 8.6 and 37 °C, respectively. Increased concentration (100 mM) of monovalent cations such as Na+ and K+ was inhibitory to the activity. Hg2+ and Zn2+ remarkably inhibited the protease activity, while Mg2+ and Ca2+ had no virtual effect. Several sulfhydryl reagents such as p-chloromercuribenzoic acid, methyl methanethiosulfonate, N-ethylmaleimide and N-phenylmaleimide also blocked the activity, confirming the previous result that cysteine residue(s) were responsible for the proteolysis. 相似文献
83.
茵栀黄注射液的内毒素检查法研究 总被引:2,自引:0,他引:2
目的:研究内毒素检查法用于茵栀黄注射液的可行性。方法:通过干扰试验,确定茵栀黄注射液对鲎试验是否具有抑制或增强作用,再对3批样品进行检测,结果:茵栀黄注射液稀释40倍,用灵敏度为0.060Eu/ml的鲎试剂检测,与热原检查结果一致,结论:内毒检查法可用于检测茵栀黄注射液中的细胞内毒素。 相似文献
84.
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86.
目的评价国产液体血凝试剂在法国Stago血凝仪上的性能。方法选择成人血浆样本285例,分别使用国产液体血凝试剂和法国Stago血凝仪原装试剂,在Stago血凝仪上进行凝血酶原时间、活化部分凝血活酶时间、纤维蛋白原和凝血酶时间4项凝血指标检测,检测结果参考美国临床实验室修正法规1988(CLIA'88)标准要求进行统计分析。结果国产液体血凝试剂的检测结果与Stago原装血凝试剂的检测结果相比,均符合美国CLIA'88标准要求,二者检测结果无显著性差异。结论国产液体血凝试剂可以代替进口原装试剂在Stago血凝仪上用于凝血4项临床实验检测。 相似文献
87.
目的探讨丙型肝炎病毒(HCV)分片段(抗-HCV-C、抗-HCV-NS3、抗-HCV-NS4、抗-HCV-NS5)试剂对抗-HCV临界(CO)范围标本的确认价值。方法酶联免疫吸附法(ELISA)方法检测抗-HCV总抗体,结果为临界值(S/CO)或灰区状态(CO±10%)的可疑标本,分离血清后贮存于-29℃低温冰箱内,集中用丙型肝炎病毒(HCV)抗体分片段酶联免疫确认试剂,在全自动酶标分析仪上进行检测,收集可疑标本44例,其中抗-HCVCO±10%阳性24例及CO±10%阴性20例。同时收集抗-HCV总抗体S/CO值大于5.0的标本30例,健康对照标本20例。结果44例抗-HCVELISA总抗体检测S/CO值为灰区状态标本中,HCV分片段确认为阳性者为22.7%(10/44),可疑者为6.8%(3/44),阴性者为70.5%(31/44)。抗-HCVCO±10%阳性中的假阳性率为54.2%(13/24),抗-HCVCO±10%阴性中的假阴性率为5.0%(1/20)。30例抗-HCV检测S/CO值大于5.0的标本中,HCV分片段确认阳性者为80.0%(24/30),可疑者为13.3%(4/30),阴性者为6.7%(2/30);20例健康对照组HCV分片段确认试验均呈阴性反应。结论用HCV分片段酶联免疫确认试剂对抗-HCVELISA总抗体检测是较好的旁证试验,特别对不确定的灰区标本进一步的确认意义甚大,可降低抗-HCV在检测低危人群时所产生的假阳性及假阴性结果,提高临床丙型肝炎诊断的准确率,对血站安全用血、避免浪费血源有一定的实用价值,且操作简便,易于推广应用。 相似文献
88.
宫腔镜联合B超诊治困难IUD取出的护理体会 总被引:1,自引:0,他引:1
宫腔镜联合B超在诊治困难宫内节育器取出中具有直观、安全、准确等优点,我院已实施50例,现汇报如下。 相似文献
89.
James Melrose Susan M. Smith Emily S. Fuller Allan A. Young Peter J. Roughley Andrew Dart Christopher B. Little 《European spine journal》2007,16(12):2193-2205
This study evaluated spatial and temporal extracellular matrix changes, induced by controlled surgical defects in the outer
third of the annulus fibrosus (AF) of ovine intervertebral discs (IVDs). Thirty-two 4 year old sheep received a 4 mm deep × 10 mm
wide standard annular surgical incision in the L1L2 and L3L4 IVDs (lesion group), 32 sheep were also subjected to the same
surgical approach but the AF was not incised (sham-operated controls). Remodeling of the IVD matrix in the lesion and sham
discs was assessed histochemically at 3, 6,12 and 26 month post operation (PO). Discs were also dissected into annular lesion
site and contra-lateral AF and NP and equivalent zones in the sham sheep group, extracted with GuHCl, dialysed, freeze dried,
digested with chondroitinase ABC/keratanase-I and aliquots examined for small leucine repeat proteoglycan (SLRP) core protein
species by Western blotting using C-terminal antibodies to decorin, biglycan, lumican and fibromodulin and monoclonal antibody
(Mab) 2B6 to unsaturated stub epitopes on chondroitin-4-sulphate generated by chondroitinase ABC. Masson Trichrome and Picrosirius
red staining demonstrated re-organisation of the outermost collagenous lamellae in the incised discs 3–6 month PO. Toluidine
blue staining also demonstrated a focal loss of anionic proteoglycan (PG) from the annular lesion 3–6 month PO with partial
recovery of PG levels by 26 month. Specific fragments of biglycan and fibromodulin were associated with remodeling of the
AF 12–26 month PO in the lesion IVDs but were absent from the NP of the lesion discs or all tissue zones in the sham animal
group. Fragments of decorin were also observed in lesion zone extracts from 3 to 6 months but diminished after this. Isolation
and characterization of the biglycan/fibromodulin fragments may identify them as prospective biomarkers of annular remodeling
and characterization of the enzyme systems responsible for their generation may identify therapeutic target molecules. 相似文献
90.
Silvio Aime Mauro Botta Valentina Mainero Enzo Terreno 《Magnetic resonance in medicine》2002,47(1):10-13
This work describes the use of [Pr-DO3A] as a shift reagent for differentiating intra- and extracellular L-lactate resonance in (1)H- and (13)C-NMR spectra. DO3A acts as heptadentate ligand towards lanthanide(III) ions, leaving two coordination vacancies for the coordination of the L-lactate ion. The exchange between free and [Pr-DO3A]-bound L-lactate is fast on the NMR timescale, thus yielding a paramagnetically shifted L-lactate signal for the substrate in the compartment containing the paramagnetic chelate. The evaluation of the method was carried out on a model system based on sealed ghosts from human red blood cells. 相似文献