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At least 865 records · Page 48Linked to original sources

[Study of peptide composition in serum albumin in patients with thyroid gland dysfunction].

Trypsin hydrolyzates of blood serum albumin of healthy people and patients with diffuse thyrotoxicosis and hypothyreosis were studied by the cellulose thin-layer electrochromatography. All the patients were found to have changes in the peptide composition of albumin trypsin hydrolyzate which resulted in disappearance of some peptides as well as in the appearance of new ones. Simultaneously conducted measurements of dispersion of optical rotation detected some changes in spectropolarimetric characteristics which provide the evidence for disperalization of its molecule. The found changes in albumin are determined by the disorder of normal protein biosynthesis and possible metabolic damage of protein.

Humans↗

[Fluorometholone Reference Standard (control 011) of National Institute of Health Sciences].

The raw material of fluorometholone was examined for the preparation of the "Fluorometholone Reference Standard (Control 011)". The analytical data obtained were: optical rotation, [alpha]20D = .5 degrees; UV spectrum, lambda max of 240 nm and specific absorbance in methanol at 240 nm = 350.7; IR spectrum, same as that of the Fluorometholone Reference Standard (Control 864); high-performance liquid chromatography (HPLC), total amount of impurities estimated to be less than 0.5%; loss on drying, 0.01%. Based on the above results, the raw material was authorized as the Fluorometholone Reference Standard (Control 011) of the National Institute of Health Sciences.

Chemical Phenomena↗

The use of deuterated analogs in qualitative and quantitative investigations of the metabolism of cyclophosphamide (NSC-26271).

Ring-deuterated analogs of cyclophosphamide (CP) (4-d2, 5-d, 4,6-d4, and 4,5,6-d6 derivatives) have been used to study the influence of deuterium substitution on the rates of metabolic pathways involving oxidation at C-4, and on the rate of elimination of acrolein from aldophosphamide. The magnitude of the deuterium isotope effect (kH/kD) associated with appropriate C-deuteration has been related to antitumor activity against the ADJ/PC6 murine plasma cell tumor. Isotope effects of 2.2 and 1.8 respectively, for the formation of 4-ketocyclophosphamide (4-keto-CP) and carboxyphosphamide, caused little or no change in antitumor activity (4-d2 and 4,6-d4 analogs compared with CP), but an isotope effect of about 5.3 for the beta-elimination pathway, consequent on 5,5-dideuteration, was paralleled by a marked drop in potency (7-13-fold increase in ED90) of 5,5-dideuterated analogs compared with that of CP. Analogs tetradeuterated in the bis(2-chloroethyl)amino function were used to quantitate CP and 4-keto-CP in human plasma and urine using stable-isotope dilution and direct-insertion electron impact mass spectrometry. The negative optical rotation of CP recovered from human urine after administration of the racemlc drug gave evidence for stereoselectivity in the metabolism.

Acrolein↗

[Chlormadinone Acetate Reference Standard (Control 881) of National Institute of Hygienic Sciences].

Chlormadinone acetate was tested for the preparation of the "Chlormadinone Acetate Reference Standard (Control 881)". Analytical data obtained were as follows: loss on drying, 0.00%; infrared spectrum, 1740, 1715, 1658, 1604, 1587, 1256, 1244 cm-1; ultraviolet spectrum, lambda max = 284 nm; absorbance, E1cm1% (284 nm) = 539-549; optical rotation, [alpha]D20: -12.1 degrees; melting point, 214.6 degrees C; thin-layer chromatography, contaminants were not detected until 300 micrograms; high-performance liquid chromatography, one contaminant was detected. On the basis of the above results, this material was authorized as the National Institute of Hygienic Sciences Reference Standard (Control 881).

Chlormadinone Acetate↗

[Effect of storage conditions on the kinetic properties of myosin ATPase].

"Substrate inhibition", which has been described earlier for myosin Ca-ATPase in low ionic strength KCl solution [1], is found to take place also at high KCl concentration and under partial modification of enzyme thiol groups with p-CMB. "Substrate inhibition" disappeared when increasing Ca2+ concentration up to 25-40 mM. These kinetic properties are characteristic for fresh isolated enzyme and myosin preparations stored in 0.5 M KCl. They may change under storage of enzyme preparations at higher KCl concentrations: no "substrate inhibition" is observed after 6-8-day storage of myosin preparations in 3 M KCl at the presence of 4-5 mM CaCl2. The data on optical rotation dispersion and analytical ultracentrifugation have shown that the storage of myosin in 3 M KCl is accompanied by structural changes of the protein.

Adenosine Triphosphatases↗

[Mestranol Reference Standard (Control 881) of National Institute of Hygienic Sciences].

The raw material of mestranol was examined for preparation of the "Mestranol Reference Standard". Analytical results for the sample were as follows: UV spectrum indicated absorption maxima at 279 and 287 nm and absorptivity at 279 nm E1%1cm 66; IR spectrum indicated specific absorption at 1612, 1578, 1505, 1253, and 1060 cm-1; optical rotation +3.9 degrees; melting point 153.1 degrees; loss on drying 0.03%; TLC and HPLC analyses indicated one impurity, respectively; the purity was assumed to be 99.3% by HPLC analysis. Based on the results, the present raw material was authorized to be the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗

[Betamethasone Sodium Phosphate Reference Standard (Control 881) of National Institute of Hygienic Sciences].

The raw material of betamethasone sodium phosphate was examined for preparation of the "Betamethasone Sodium Phosphate Reference Standard". Analytical results for the sample were as follows: pH 7.90; optical rotation + 100.5 degrees; IR spectrum the same as USP Reference Standard of Betamethasone Sodium Phosphate; TLC indicated no impurities, but 5 kinds of impurities were detected in small amounts by HPLC; water content 14.7%; assay 100.2% by HPLC. Based on the above results, this raw material was authorized to be the Reference Standard of the National Institute of Hygienic Sciences.

Betamethasone↗

[Dexamethasone Sodium Phosphate Reference Standard (Control 891) of National Institute of Hygienic Sciences].

The raw material of dexamethasone sodium phosphate was examined for preparation of the "Dexamethasone Sodium Phosphate Reference Standard". Analytical results were as follows: UV spectrum indicates absorption maxima at 242 nm and absorptivity at 242 nm is E1%1cm 304; optical rotation +79.0%; pH 7.7; ethanol 5.2%; water 6.0%; HPLC analysis indicates small amounts of three impurities and the purity was assumed to be 99.8%; assay by HPLC indicated 100.9% against the USP Reference Standard of "Dexamethasone Phosphate". Based on the results, the present raw material was authorized to be the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗

[Hydrocortisone Acetate Reference Standard (Control 891) of National Institute of Hygienic Sciences].

The raw material of hydrocortisone acetate was examined for preparation of the "Hydrocortisone Acetate Reference Standard". Analytical results were as follows: E1%1cm (242 nm) 403; IR spectrum indicates specific absorption at 3424, 1745, 1721, 1630, and 1374 cm-1; optical rotation +164.4 degrees (in dioxane); melting point 219.5 degrees (decomposition); loss on drying 0.16%; TLC and HPLC analyses indicated one and three impurities, respectively; assay by HPLC was 99.7% against the previous Reference Standard. Based on the results, the present raw material was authorized to be the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗

[Hydrocortisone Sodium Phosphate Reference Standard (Control 891) of National Institute of Hygienic Sciences].

The raw material of hydrocortisone sodium phosphate was examined for the preparation of the "Hydrocortisone Sodium Phosphate Reference Standard". Analytical data obtained were as follows: pH, 8.2; optical rotation [alpha]D20, +124.1 degrees; Infrared spectrum, same as that of BP Reference Standard of Hydrocortisone Sodium Phosphate; thin-layer chromatography, no impurities were detected; high-performance liquid chromatography (HPLC), 2 kinds of small amount of impurities were detected; assay, 99.2% by the enzyme method and 99.9% by the HPLC method in terms of the BP Reference Standard. Based on the above results, this raw material was authorized to be the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗

[Prednisolone Sodium Phosphate Reference Standard (Control 891) of National Institute of Hygienic Sciences].

The raw material of prednisolone sodium phosphate was examined for preparation of the "Prednizolone Sodium Phosphate Reference Standard". Analytical data obtained were as follows: pH 7.6; optical rotation [alpha]D25, +99.0 degrees; Infrared spectrum, same as that of BP Reference Standard; Thin-layer chromatography, 4 impurities were detected; high-performance liquid chromatography (HPLC), 7 kinds of impurities were detected; residual solvent, 0.76% (ethnol) and 0.23% (hexane); assay, 100.2% by the enzyme method and 99.7% by the HPLC method in terms of the BP Reference Standard. Based on the above results, this raw material was authorized to be the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗

[Methyldigoxin Reference Standard (Control 881) of National Institute of Hygienic Sciences].

Methyldigoxin was tested for preparation of the "Methyldigoxin Reference Standard (Control 881)". Analytical data obtained were as follows: infrared spectrum 3456, 1738, 1086 cm-1; ultraviolet spectrum lambda max = 219 nm; absorbance E1cm1% (219 nm) = 193.1; water 0.99%; optical rotation [alpha]546.1(20) = +22.5 degrees; thin-layer chromatography and high-performance liquid chromatography indicates two impurities, respectively; quantitative analysis of acetone 3.87%; assay by spectrophotometry 100.3% against Digoxin Reference Standard (Control 802). On the basis of the above results, this material was authorized as the National Institute of the Hygienic Sciences Reference Standard (Control 881).

Chromatography, High Pressure Liquid↗

[Cholecalciferol Reference Standard (Control 901) of the National Institute of Hygienic Sciences].

Cholecalciferol Reference Standard for the Japanese Pharmacopoeia (JP RS) was prepared. The following analytical data were obtained: melting point 85.8 degrees C; UV and IR spectra were in agreement with both of the previous JP RS and USP RS of Cholecalciferol; absorptivity at 265 nm E1%lcm = 476; optical rotation [alpha]20D = + 110.1 degrees; no impurities were detected by TLC and HPLC analyses; assay 100.1% by HPLC against the USP RS. Based on the above results, the raw material was authorized as the Reference Standard of the National Institute of Hygienic Sciences.

Cholecalciferol↗

[Ergocalciferol Reference Standard (Control 901) of the National Institute of Hygienic Sciences].

Ergocalciferol Reference Standard for the Japanese Pharmacopoeia (JP RS) was prepared. The following analytical data were obtained: melting point 118.4 degrees C; UV and IR spectra were in agreement with both of the previous JP RS and USP RS of ergocalciferol; absorptivity at 265nm E1%lcm = 467; optical rotation [alpha]20D = 103 degrees; no impurities were detected by TLC and HPLC analyses; assay 100.1% by HPLC against the USP RS. Based on the above results, the raw material was authorized as the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗

[Prednisolone Acetate Reference Standard (Control 901) of the National Institute of Hygienic Sciences].

Prednisolone Acetate Reference Standard (Control 901) for the Japanese Pharmacopoeia (JP RS) was prepared. The following analytical data were obtained: melting point 236 degrees C (decomposition); IR spectrum was same as that of JP RS of prednisolone acetate; absorptivity at 243 nm E1%lcm = 379; optical rotation [alpha]20D = +113.0 degrees; no impurity was detected by TLC, but a small amount of two impurities was found by HPLC analysis; assay by HPLC against the JP RS 100.2%. Based on the above results, this raw material was authorized as the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗

[Fluocinolone Acetonide Reference Standard (Control 901) of the National Institute of Hygienic Sciences)].

Fluocinolone Acetonide Reference Standard (Control 901) for the Japanese Pharmacopoeia (JP RS) was prepared. The following analytical data were obtained: melting point 268 degrees C (decomposition); IR spectrum was same as the previous JP RS of Fluocinolone Acetonide; absorptivity at 237nm E1%1lcm = 363; optical rotation [alpha]20D = 105.7 degrees; no impurity was detected by TLC, but two impurities were detected by HPLC analysis; assay by HPLC against the previous JP RS 100.2%. Based on the above results, this raw material was authorized as the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗

[Epitiostanol Reference Standard (Control 891) of National Institute of Hygienic Sciences].

The raw material of epitiostanol was examined for preparation of "Epitiostanol Reference Standard". Analytical results for the sample were as follows: melting point 130.7 degrees C (decomposition); UV spectrum indicates absorption maximum at 263 nm in ethanol; IR spectrum indicates specific absorption at 2920, 1383, 1056 and 590 cm-1; optical rotation [alpha]20D+ 24.4 degrees; no impurity was found by TLC, but a small amount of one was found by HPLC analysis and the purity is assumed to be 99.5%; water content 1.52%. Based on the results, the present raw material was authorized to be the Reference Standard of the National Institute of Hygienic Sciences.

Androstanols↗

[Methylergometrine Maleate Reference Standard (Control 891) of National Institute of Hygienic Sciences].

The raw material of methylergometrine maleate was examined for the preparation of the "Methylergometrine Maleate Reference Standard". Analytical data obtained were as follows: melting point, 181.7 degrees C; ultraviolet spectrum, lambda max = 313 nm; absorbance, E1%1cm (313 nm) = 181.3; infrared spectrum, 3406, 2962, 2928, 1645, 1574 cm-1; thin-layer chromatography, 6 impurities were detected; high-performance liquid chromatography, no impurities were detected; loss on drying, 0.02%; optical rotation, [alpha]20D = + 44.04 degrees; assay, 99.5% against Ergometrine Maleate Reference Standard (Control 755). Based on the above results, this raw material was authorized to be the Reference Standard of the National Institute of Hygienic Sciences.

Chromatography, High Pressure Liquid↗