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Ten benzodiazepines--clorazepate, nitrazepam, clonazepam, oxazepam, lorazepam, chlordiazepoxide, N-desmethyldiazepam, diazepam, prazepam, and flurazepam--in solid dosage form are identified by ultraviolet (UV) and infrared (IR) spectrophotometry and by high pressure liquid chromatography (HPLC). UV absorption data and IR spectra of the 10 benzodiazepines are provided and HPLC separation methods are described.
Numerous methods can be used for the analysis of urinary stones, but few of them provide information on the structure, chemical composition and crystal phases of these stones. In a good urinary stone analysis the stone is first examined through a binocular magnifying glass, for instance, to detect its structural features including umbilication. Randall's plaque, bracketing faces and individualized or non-individualized nucleus. Morphological typing is important as it points to one pathology or another irrespective of composition. Composition must be determined quantitatively, with differentiation of crystal phases, and this requires global physical methods such as X-ray microdiffractiometry or infrared spectrophotometry. Urinary crystals can be identified by polarized light microscopy supplemented, if necessary, by infrared microscopy when the crystals are few and of unusual morphology. Studying crystalluria is a simple and efficient means of following up lithiasic patients, provided their urine is collected and stored under adequate conditions. In interpreting the results various criteria, and particularly the nature, abundance, size, facies, aggregation and frequency of crystals, must be taken into account.
UNLABELLED: Near-infrared spectrophotometry assesses cerebral oxygen saturation (ScO(2)) based on the absorption spectra of oxygenated and deoxygenated hemoglobin and the translucency of biological tissue in the near-infrared band. In patients with icterus, however, bilirubin can potentially hinder cerebral oximetry. In 48 patients undergoing orthotopic liver transplantation, we related total plasma bilirubin to ScO(2) as determined from spectrophotometry with wavelengths of 733 and 809 nm. Before surgery, ScO(2) was 59% (15%-78%) (median with range) and bilirubin was 71 (6-619) micromol/L with a negative correlation (r = -0.72; P < 0.05). The 95% prediction interval included the lowest measurable ScO(2) of 15% at a bilirubin level of 370 micromol/L. During reperfusion of the grafted liver, the ScO(2) increased by 7% (-8% to 17%) (P < 0.05), and bilirubin did not influence this increase. In one patient, the ScO(2) remained below 15% despite a decrease in bilirubin from 619 to 125 micromol/L, suggesting that tissue pigmentation deposits also absorb light. In conclusion, bilirubin dampens the spectrophotometry-determined cerebral oxygen saturation at 733 and 809 nm. A bilirubin level of 370 micromol/L, tissue pigment deposits, or both, may render determination of cerebral oxygen saturation impossible. Even at high bilirubin values, changes in cerebral perfusion may be visible. IMPLICATIONS: In 48 patients undergoing liver transplantation, the interference of icterus on cerebral oximetry by near-infrared light was investigated. Bilirubin absorbed the near-infrared light and lowered the measured cerebral oxygen saturation. Even at high bilirubin values, changes in cerebral oxygenation, as seen during reperfusion of the grafted liver, may be visible.
For the purpose of detecting fetal pulmonary maturity with real-time convenience but reliable accuracy, infrared spectrophotometry of amniotic fluid lipids was introduced using our newly developed optical device. The peak areas at the wave number of 1740 cm-1 on the infrared spectra (called "PA1740") were measured in 29 specimens sampled from 29 pregnant women, and compared with the Lecithin/Sphingomyelin (L/S) ratio of the same samples. Statistical analysis revealed that the PA1740 was almost as reliable as the L/S ratio, and these indices illustrated pulmonary immaturity in cases with a PA1740 less than 0.9 and an L/S ratio less than 2.0. PA1740 is absolutely independent of the effect on the concentration of lecithin in the amniotic fluid because of a combination of the vacuum-drying process and the absorbance correction, and can be completed in less than 20 minutes from sampling of the amniotic fluid by a very simple manipulation. In conclusion, the new index, PA1740, will be a more practical method for prediction of the fetal pulmonary maturity than methods such as the well known L/S ratio.
In order to determine the effects of age on bone quality, human bone tissue taken from adult subjects deceased from violent death was analyzed by means of fast Fourier transform infrared spectrophotometry (FTIR) in the Diffuse Reflectance mode (DR). This technique allows the characterization of both the mineral and organic parts of bone in a nondestructive manner. Only the organic part is discussed in this report. A quantitative change in the entire organic part of bone tissue is observed with the aging of subjects. The effects of these changes on bone strength were not measured.
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Antigenic extracts of Streptococcus group E (SGE) were subjected to fractional ethanol precipitation, block (preparative) electrophoresis, and gel filtration for the purpose of separating the type antigen from the group antigen. Ethanol precipitation was ineffective in separating the substances. Block electrophoresis yielded serologically pure group antigen and a mixture of type and group antigen. Serologically pure type antigen was obtained by gel filtration. In some cases, pure group antigen was also recovered; in others, it was contaminated with type antigen. Gel filtration column effluents of antigenic extracts of SGE serotypes, I, II, III, IV, V and "untypable" isolates, collected from the region in which type antigen was eluted, were studied by paper chromatography and infrared spectrophotometry in an effort to develop a nonserological means of detecting type antigen. Hydrolysates of type antigens or suspect type antigens of serotypes I through V contained l-rhamnose, d-glucose, and several unidentified substances. d-Galactose also was present in hydrolysates of serotypes III and V. Untypable isolates and negative controls contained traces of d-glucose only. The data suggested that serotypes I through V contained a type antigen and that the untypable isolates were devoid of type antigen. Infrared absorbance spectra seemed to support the paper chromatography data.
A further cytochalasin was isolated from liquid culture filtrates of Phoma exigua var. heteromorpha together with cytochalasins U and V and other well-known cytochalasins. The metabolite, named cytochalasin W, was characterized by spectroscopic and chemical methods as a new 24-oxa[14]cytochalasan, bearing a formyl group on the macrocyclic ring. Cytochalasin W showed toxic activity in the brine shrimp assay.
Mononuclear trivalent lanthanide complexes with formula [Ln(L)(NO(3))(3)] [in which L=4,4-difluoro-8-(2':2'';6'':2'''-terpyridin-4''-yl)-1,3,5,7-tetramethyl-2,6-diethyl-4-bora-3a,4a-diaza-s-indacene (Boditerpy)] are reported for Ln=Yb, Nd, Er, La and Gd. According to the crystal structure of the Yb complex, the lanthanide ion is bound to the terdentate terpyridine and the inner coordination sphere of the nine-coordinate lanthanide ion is completed by three bidentate nitrate anions. The coordination polyhedron can be described as a distorted tricapped antiprism. The terpyridine chelate is almost planar and tilted by nearly 60 degrees from the indacene subunit. FT-IR spectra confirm the bidentate binding mode of the nitrate anions for the other complexes. NMR and ES-MS spectra (through characteristic isotopic patterns) confirm the chemical formulation. The complexes have high molar absorption coefficients in the visible spectral region (65,000 M(-1) cm(-1) at 529 nm) and display sizeable NIR luminescence (900 to 1600 nm, for Ln=Yb, Nd and Er), upon irradiation through the electronic state of the indacene moiety at 514 nm. Crystal-field splitting was analysed at low temperature. The quantum yield of the Yb solution (10(-4) M) in dichloromethane amounts to 0.31 %, corresponding to a sensitisation efficacy of the ligand of ca. 63 %.
In a bioassay guided phytochemical investigation of Toona ciliata (Fam. Meliaceae), a new hydroxy steroidal ketone, 12alpha-hydroxystigmast-4-en-3-one (1) was isolated from the petroleum ether extract of the plant together with two known steroids and three C-methyl coumarins. The structure of 1 was established by means of spectroscopic analyses. Compound 1 was found cytotoxic in a brine shrimp lethality bioassay with LC50 of 9.9 microg/ml and it also showed significant antitumor activity with Ti50 value of 14.1 microg/ml in a potato disc bioassay.
Twelve compounds with lipid peroxidation inhibitory activity were isolated from the stem bark of E. globulus. Their structures were assigned as a new aromatic monoterpene (1) and eleven known compounds, pinoresinol (2), vomifoliol (3), 3,4,5-trimethoxyphenol 1-O-beta-D-(6'-O-galloyl)glucopyranoside (4), methyl gallate (5), rhamnazin (6), rhamnetin (7), eriodictyol (8), quercetin (9), taxifolin (10), engelitin (11), and catechin (12) on the basis of UV, mass, and NMR spectroscopic analyses. These compounds except vomifoliol significantly inhibited lipid peroxidation in rat liver microsome.
A new stilbene diglycoside, piceatannol-3, 4'-O-beta-D-diglucopyranoside (I), together with desoxyrhaponticin (II), emodin-1-O-beta-D-glucopyranoside (III), and physcion-8-O-b-D-glucopyranoside (IV), were isolated from the rhizomes of cultivated Korean rhubarb rhizomes (Rheum undulatum), Jong DaeWhang, and the structures of I-IV were identified on the basis of chemical and spectral evidences.
Cytotoxic and antimutagenic effects of a novel cis-epsilon-viniferin and five known stilbenes, transresveratrol, trans-epsilon-viniferin, gnetin H, suffruticosols A and B, isolated from the seeds of Paeonia lactiflora Pall. (Paeoniaceae) were determined against five different cancer cell lines, and mutagenicity of N-methyl-N'-nitro-N-nitrosoguanidine (MNNG) in Salmonella typhimurium TA100, respectively. Six stilbenes showed cytotoxic activity in a dose-dependent manner, and especially did potent cytotoxic activity against C6 (mouse glioma) cancer cell with IC50 values ranging from 8.2 to 20.5 microg/ml. trans-Resveratrol showed significant cytotoxic activity against HepG2 (liver hepatoma) and HT-29 (colon) human cancer cell lines with IC50 values of 11.8 and 25.2 g/ml, respectively. In contrast, trans-epsilon-viniferin and cis--viniferin, and gnetin H exhibited marked cytotoxic activity against Hela (cervicse) and MCF-7 (breast) human cancer cell lines with IC50 values of 20.4, 21.5, and 12.9 microg/ml, respectively. However, suffruticosol A and B had less cytotoxic effect against all cancer cells except C6. Meanwhile, six stilbenes exerted antimutagenic activity in a dose-dependent fashion. Of them, trans-resveratrol exhibited the strongest antimutagenic effect against MNNG with IC50 value of 27.0 microg/plate, while other five resveratrol oligomers also did moderate antimutagenic activity with IC50 values ranging from 31.7 to 35.2 microg/plate.
A total of eight flavonoids (1-8), including a novel quercetin-7-O-(6''-O-acetyl)-beta-D-glucopyranoside (6) and seven known flavonoids, luteolin (1), quercetin (2), luteolin 7-O-beta-D-glucopyranoside (3), luteolin-7-O-(6''-O-acetyl)-beta-D-glucopyranoside (4) quercetin 7-O-beta-D-glucopyranoside (5), acacetin 7-O-beta-D-glucuronide (7) and apigenin-6-C-beta-D-glucopyrano syl-8-C-beta-D-glucopyranoside (8), have been isolated from the leaves of the safflower (Carthamus tinctorius L.) and identified on the basis of spectroscopic and chemical studies. The antioxidative activity of these flavonoids was evaluated against 2-deoxyribose degradation and rat liver microsomal lipid peroxidation induced by hydroxyl radicals generated via a Fenton-type reaction. Among these flavonoids, luteolin-acetyl-glucoside (4) and quercetin-acetyl-glucoside (6) showed potent antioxidative activities against 2-deoxyribose degradation and lipid peroxidation in rat liver microsomes. Luteolin (1), quercetin (2), and their corresponding glycosides (3 & 5) also exhibited strong antioxidative activity, while acacetin glucuronide (7) and apigenin-6,8-di-C-glucoside (8) were relatively less active.
Activity-guided fractionation of the EtOAc-soluble extract of the stems of Couepia ulei, using a bioassay based on the induction of quinone reductase (QR) in cultured Hepa 1c1c7 mouse hepatoma cells led to the isolation of two active compounds, a new natural product, erythro-2,3-bis(4-hydroxy-3-methoxyphenyl)-3-ethoxypropan-1-ol (1), and a known compound, evofolin-B (2), along with five inactive compounds all of known structure, viz., betulinic acid, oleanolic acid, pomolic acid, (+/-)-syringaresinol, and ursolic acid. These isolates were identified by analysis of physical and spectral data. Compounds 1 and 2 exhibited QR inducing activity, with observed CD (concentration required to double induction) values of 16.7 and 16.4 microM, respectively.
We have designed and synthesized new optically active bisviologens ([BNMV](4+)) containing a binaphthyl moiety to examine the stereoselective photoinduced electron-transfer (ET) reactions with zinc-substituted myoglobin (ZnMb) by flash photolysis. The photoexcited triplet state of ZnMb, (3)(ZnMb)*, was successfully quenched by [BNMV](4+) ions to form the radical pair of a ZnMb cation (ZnMb(.+)) and a reduced viologen ([BNMV](.3+)), followed by a thermal ET reaction to the ground state. The rate constants ( k(q)) for the ET quenching at 25 degrees C were obtained as k(q)( R)=(2.9+/-0.2)x10(7) M(-1) s(-1) and k(q)( S)=(2.2+/-0.2)x10(7) M(-1) s(-1), respectively. The ratio of k(q)( R)/ k(q)( S)=1.3 indicates that the ( R)-isomer of the chiral viologen preferentially quenches (3)(ZnMb)*. On the other hand, the rate constants ( k) for the thermal ET reaction from [BNMV](.3+) to ZnMb(-+) at 25 degrees C were k( R)=(1.2+/-0.1)x10(8) M(-1) s(-1) and k( S)=(0.47+/-0.03)x10(8) M(-1) s(-1), respectively, and the ratio remarkably increased to k( R)/ k( S)=2.6. The activation parameters, Delta H(not equal) and Delta S(not equal), were determined from the kinetic measurements at various temperatures (10-30 degrees C) to understand the ET mechanisms. In the quenching reaction, the energy differences of Delta Delta H*(R- S) and T Delta Delta S*( R- S) at 25 degrees C were calculated to be -3.9+/-1.6 and -3.3+/-0.2 kJ mol(-1), respectively, whereas Delta Delta H*( R-S)=7.7+/-1.9 kJ mol(-1 )and T Delta Delta S*( R-S)=9.9+/-0.5 kJ mol(-1 )were found for the thermal ET reaction. Therefore, the thermal ET reaction to the ground state was proved to be dominated by the entropy term, and the large stereoselectivity may arise from the decrease in charge repulsion between donor and acceptor.
An amphiphilic graft polyphosphazene (PNIPAm/EAB-PPP) composed of oligo-poly(N-isopropylacrylamide) (PNIPAm) as hydrophilic segments and ethyl 4-aminobenzoate (EAB) as hydrophobic groups was synthesized via ring-opening polymerization and subsequent substitution reaction. The molar ratio of the PNIPAm segment to EAB group was 1.85:0.15. The lower critical solution temperature (LCST) of copolymer was 32.6 degrees C as determined by turbidity method. Micellization behavior of PNIPAm/EAB-PPP in an aqueous phase was characterized by fluorescence technique, 1H NMR, dynamic light scattering (DLS) and transmission electron microscopy (TEM). The critical micelle concentration (CMC) of the graft copolymer in aqueous solution was 0.1mg/ml. The number-averaged particle size of spherical micelles was 80 nm at 25 degrees C with a narrow distribution. TEM also revealed that inter-micellar aggregation was induced in the micelle solution at temperature above LCST of graft copolymer. The thermosensitive PNIPAm/EAB-PPP micelles may be of help to regulate the loading and release of hydrophobic drugs.
The synthesis of a new series of 1beta-methylcarbapenems having methoxyimine and substituted sulfonamide moieties is described. Their in vitro antibacterial activities against both Gram-positive and Gram-negative bacteria were tested and the effect of substituents on the pyrrolidine ring was investigated. A particular compound (IIIc) having methylaminosulfonamide moiety showed the most potent antibacterial activity.