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Various flavianic acids were prepared and examined for the preparation for color reference standard for thin-layer chromatography (TLC). Their analytical data were: IR spetra, their specific absorptions were same; no impurities were detected; specific odor-free. It was clear that the prepared flavianic acids were useable as color reference standards for TLC.
The raw material of tocopherol was tested for the preparation of "Tocopherol Reference Standard (Control 991)". Analytical data obtained were: IR spectrum, same as the Tocopherol Reference Standard (Control 941); specific absorbance, E/cm% (292 nm) = 72.9; thin-layer chromatography, no impurities were detected until 50.0 micrograms; high-performance liquid chromatography (HPLC), trace amounts of five impurities were detected and the total amount was estimated to be less than 1.4%; assay by HPLC, 99.9%. Based on the above results, the raw material was authorized as the Japanese Pharmacopoeia Standard (Control 991).
Two new standard reference materials (SRM) for drugs of abuse in human hair have been developed. SRM 2379 consists of hair spiked with cocaine, benzoylecgonine, cocaethylene, phencyclidine, amphetamine, and methamphetamine. SRM 2380 consists of hair spiked with codeine, morphine, monoacetylmorphine, and tetrahydrocannabinol (THC). The SRMs were prepared by soaking the hair in a solution of the target analytes in water-dimethylsulfoxide. The concentration of each analyte was determined using two methods, one based upon gas chromatography/mass spectrometry (GC/MS) and one based upon liquid chromatography/mass spectrometry (LC/MS). Both methods used 0.1 M HCl for extraction of all the analytes from the hair, except for THC, which was extracted with 1 M NaOH. For isolation of the analytes from the extracts, the GC/MS-based methods used different clean-up procedures from those used for the LC/MS-based methods. The results from the two methods were in good agreement with mean differences for the analytes ranging from 4% to 16%. These materials will enable laboratories performing analyses of hair for drugs of abuse to test the accuracy of their methods.
A number of food-matrix reference materials (RMs) are available from the National Institute of Standards and Technology (NIST) and from Agriculture Canada through NIST. Most of these materials were originally value-assigned for their elemental composition (major, minor, and trace elements), but no additional nutritional information was provided. Two of the materials were certified for selected organic constituents. Ten of these materials (Standard Reference Material [SRM] 1,563 Cholesterol and Fat-Soluble Vitamins in Coconut Oil [Natural and Fortified], SRM 1,566b Oyster Tissue, SRM 1,570a Spinach Leaves, SRM 1,974a Organics in Mussel Tissue (Mytilus edulis), RM 8,415 Whole Egg Powder, RM 8,418 Wheat Gluten, RM 8,432 Corn Starch, RM 8,433 Corn Bran, RM 8,435 Whole Milk Powder, and RM 8,436 Durum Wheat Flour) were recently distributed by NIST to 4 laboratories with expertise in food analysis for the measurement of proximates (solids, fat, protein, etc.), calories, and total dietary fiber, as appropriate. SRM 1846 Infant Formula was distributed as a quality control sample for the proximates and for analysis for individual fatty acids. Two of the materials (Whole Egg Powder and Whole Milk Powder) were distributed in an earlier interlaboratory comparison exercise in which they were analyzed for several vitamins. Value assignment of analyte concentrations in these 11 SRMs and RMs, based on analyses by the collaborating laboratories, is described in this paper. These materials are intended primarily for validation of analytical methods for the measurement of nutrients in foods of similar composition (based on AOAC INTERNATIONAL's fat-protein-carbohydrate triangle). They may also be used as "primary control materials" in the value assignment of in-house control materials of similar composition. The addition of proximate information for 10 existing reference materials means that RMs are now available from NIST with assigned values for proximates in 6 of the 9 sectors of the AOAC triangle. Five of these materials have values assigned for total dietary fiber-the first such information provided for materials available from NIST.
A total of 128 previously frozen first-void urine (FVU) specimens from selected asymptomatic men were centrifuged and tested by three Chlamydia trachomatis rapid antigen detection tests and with a leukocyte esterase (LE) dipstick. When the results were compared to those of a reference standard of positivity determined by the Chlamydiazyme enzyme immunoassay as confirmed by a blocking assay, the sensitivities of the Testpack Chlamydia (Abbott), Clearview Chlamydia (Unipath), and Surecell Chlamydia (Kodak) tests and the LE dipstick test were 76.4, 76.4, 67.3, and 88.6%, respectively. Use of the ligase chain reaction (LCR), whose results were confirmed by direct fluorescent-antibody staining of elementary bodies, as the reference standard reduced the sensitivities to 70.9, 67.7, 62.9, and 87.5%, respectively. The specificities by use of LCR as the reference standard were 95.5, 95.5, 100, and 92.4%, respectively. These rapid chlamydial antigen tests performed reasonably well with FVU specimens, but the simple LE dipstick test, which had the highest sensitivity, would have enabled treatment of the greatest number of infected male patients.
The procedural standard for DNA profiling developed by the U.S. advisory board on DNA quality assurance methods mandates annual confirmation of forensic DNA measurement systems against an appropriate reference material supplied by or traceable to the National Institute of Standards and Technology (NIST). NIST Standard Reference Material (SRM) 2390 is a suitable and appropriate standard for HaeIII restriction enzyme-based restriction fragment length polymorphism (RFLP) profiling systems. Originally issued in 1992, an among-laboratory SRM 2390 recertification study was initiated in 1997. Using data provided by the 20 state, local, or commercial forensic laboratory participants, quantitative band sizes values (expected mean values and associated bivariate tolerance intervals) are established for two different-source DNAs (female cell line K562 and healthy male "TAW") for genetic loci D1S7, D2S44, D4S139, D5S110, D1OS28, and D17S79. Methods for validating an RFLP measurement system, validating a control material or other secondary standard, and for tracing a particular set of RFLP measurements to NIST SRM 2390 are described in detail.
Observations made during biochemical and toxicological studies of the housefly, in which the WHO standard reference (SR) strain was used as a standard, indicated that this strain differs from other strains in certain physiological and toxicological aspects. Experiments are described in which microsomal oxidases prepared from the standard reference strain and several other housefly strains, both susceptible and resistant to insecticides, were compared for heat stability, sensitivity to ionic strength, pH optima, and the spectral characteristics of their cytochrome P-450. In a comparison with 8 strains the SR strain microsomes were more stable at high incubation temperatures (40-47.5 degrees C). Compared to two other strains (NAIDM, susceptible, and Isolan-B, resistant) SR was more stable at low pH and more sensitive to high ionic strength. In spectral comparisons with NAIDM and Isolan-B, SR was found to contain microsomal cytochrome P-450 that differed slightly in its carbon monoxide or octylamine binding spectra. The results suggest that this strain may not provide a suitable reference in studies involving the microsomal oxidases. However, these apparent differences should not reduce the value of the SR stain as a reference in insecticide resistance studies.
Standard reference materials (SRM) made of polyurethane films containing various amounts of cytotoxic compounds such as zinc diethyldithiocarbamate (ZDEC) and zinc dibutyldithiocarbamate (ZDBC) are proposed. The cytotoxicity indices of five dithiocarbamates and the SRM films obtained by colony assay were compared with those by published standards, i.e., neutral red assay (NF S 90-702), agar diffusion assay (USP XXII), and millipore filter diffusion assay (DIN-V 13 930). Among them, colony assay using 3 cell lines of Balb 3T3, L929 and V79 was found to be most sensitive. The extraction method and direct contact method were proposed as two test methods of colony assay. In the former, culture media after incubation with test materials were used as test solution, and in the latter, cells were directly cultured on test materials. The extraction method gave a linear relationship between the cytotoxic potentials of the SRM and its concentration of ZDEC or ZDBC. The cytotoxic potentials of the SRM correlated well with the thickness of inflammatory layer in rabbit muscle implantation tests of the SRM. The direct contact method was found to be useful to detect weak cytotoxicity because of its high sensitivity. Based on these data, we propose the colony assay and the two kinds of new SRMs as Japanese standard test method for evaluating the cytotoxicity of biomaterials.
The United States Pharmacopeia (USP) is a private standards-setting body created in 1820 by practitioners who wished to promote the quality of therapeutic products in commerce. The principal product of USP, then and now, is the United StatesPharmacopeia (USP), to which was added the National Formulary (NF) in 1975. The two compendia are published as a combined text annually (USP-NF). Originally a book of process standards, USP-NF evolved over time into compendia containing primarily product standards that are expressed in monographs for therapeutic ingredients, products, and excipients. As a public health service, USP supplies official USP Reference Standards to manufacturers and others who wish to test an article according to selected procedures of a monograph or General Chapter. During the past decade, understanding of USP monographs and official USP Reference Standards as a means of controlling the quality of a therapeutic article has evolved, based on advances in metrology, on activities in the International Conference on Harmonization of Technical Requirements for the Registration of Pharmaceuticals for Human Use (ICH), and on considerations by the USP Council of Experts and its Expert Committees and USP staff. This article discusses the evolution of this understanding, focusing on drug substances and excipients for well-characterized small molecules and their corresponding dosage forms.
Although often used as a reference standard in the breath hydrogen test (BHT), lactulose fermentation produces more hydrogen, compared to starch, and may therefore not be ideal. This study compares inulin with lactulose as reference standard in the study of carbohydrate malabsorption. Seventeen patients with malabsorption due to chronic pancreatitis and 15 normal controls were studied. Following overnight fasts, BHTs were performed after ingesting 10 g lactulose, 10 g inulin, and 200 g (16 g highly resistant starch) maize meal. Lactulose fermentation produced significantly more hydrogen than inulin in patients with malabsorption (97 +/- 20 vs 45 +/- 22 ppm x hr; P < 0.05) and controls (43 +/- 18 vs 21 +/- 10 ppm x hr; P < 0.05). Patients produced more hydrogen than controls with both standards (lactulose, 97 +/- 20 vs 43 +/- 18 ppm x hr, P < 0.05; inulin 45 +/- 22 vs 21 +/- 10 ppm x hrs; P < 0.05), suggesting adaptation of the colonic flora. Calculated CHO malabsorption was 2.5 +/- 0.8 vs 5.2 +/- 3.8 g with lactulose and 5.2 +/- 3.1 vs 11.2 +/- 9.6 g with inulin as standards in controls and patients, respectively (P < 0.05). Lactulose produces more breath hydrogen than inulin. Calculation of CHO malabsorption using these standards is therefore not comparable.
The raw material of paeoniflorin was examined for preparation of the "Paeoniflorin Reference Standard". The analytical data obtained were: UV spectrum: lambda max, 231.7 nm; and specific absorbance (E1% 1 cm) in methanol at 230 nm, 265.4; IR spectrum, specific absorptions of raw material were consistent with that of Standard (Control 985). High-performance liquid chromatography, several impurities were detected. The amount of each impurity was estimated at less than 0.1% and total amount of impurities was less than 0.2%. Based on the above results, the candidate material was authorized as the Paeoniflorin Reference Standard (Control 011) of the National Institute of Health Sciences.
The raw material of thiamine hydrochloride was examined for preparation of the "Thiamine Hydrochloride Reference Standard". The analytical data obtained were: assay by HPLC, 100.5%; spectrophotometric assay 101.2%. Based on the above results, the candidate material was authorized as the Thiamine Hydrochloride Reference Standard (Control 021) of the National Institute of Health Sciences.
The raw material of triamcinolone was examined for preparation of the "Triamcinolone Reference Standard (Control 981)". The analytical data obtained were: melting point, 246 degrees C (decomposition); UV spectrum, lambda max of 239 nm and specific absorbance in methanol at 289 nm of 394; IR spectrum, specific absorptions at 3462, 1716, 1659, 1615, 1604, 1132 and 1061 cm-1; optical rotation, [alpha]D20 = +69.7 degrees; high-performance liquid chromatography, five impurities detected and amount of each impurity estimated to be less than 0.6% and total amount of impurities less than 1.4%; loss on drying, 0.24%. Based on the above results, the raw material was authorized as the Triamcinolone Reference Standard (Control 981) of the National Institute of Health Sciences.
Diflucortolone-21-valerate was tested for the preparation of "Diflucortolone-21-valerate Reference Standard (Control 871)". Analytical data obtained were as follows: loss on drying, 0.05%; infrared spectrum, 1745, 1727, 1667, 1625, 1611, 1169 cm-1; ultraviolet spectrum, lambda max = 239 nm; absorbance, E1%1cm (239 nm) = 348.8; optical rotation, [alpha]20D: + 100.8 degrees; melting point, 203.2 degrees C; thin-layer chromatography, three contaminants were detected; high-performance liquid chromatography, two contaminants were detected; fluorine, 8.06%. On the basis of those results, this material was authorized as the National Institute of Hygienic Sciences Reference Standard (Control 871).
AIMS: To use BioBall cultures as a precise reference standard to evaluate methods for enumeration of Escherichia coli and other coliform bacteria in water samples. METHODS AND RESULTS: Eight methods were evaluated including membrane filtration, standard plate count (pour and spread plate methods), defined substrate technology methods (Colilert and Colisure), the most probable number method and the Petrifilm disposable plate method. Escherichia coli and Enterobacter aerogenes BioBall cultures containing 30 organisms each were used. All tests were performed using 10 replicates. The mean recovery of both bacteria varied with the different methods employed. CONCLUSIONS: The best and most consistent results were obtained with Petrifilm and the pour plate method. Other methods either yielded a low recovery or showed significantly high variability between replicates. SIGNIFICANCE AND IMPACT OF THE STUDY: The BioBall is a very suitable quality control tool for evaluating the efficiency of methods for bacterial enumeration in water samples.
The Kellgren and Lawrence atlas has been the reference standard for radiographic classification of osteoarthritis (OA) for nearly 40 years. Limitations include employment of a global grade, over-emphasis of the osteophyte, and submergence of other features so measurement of disease progression is difficult. Observer bias, drift, and variability cause concern. To address deficiencies and optimize observer accuracy, precision, and agreement, an updated atlas was created. From a photographic set of clinical radiographs, 4 readers selected a subset by consensus. Major radiographic features of hand, hip, and knee OA are graded on a 4-point scale. Using this atlas, it should be possible to individually score each relevant feature in a given joint. It is hoped the atlas will be adopted for population studies, assessment of disease progression, and protocols that evaluate new agents capable of modifying disease.
The raw material of glycyrrhizic acid examined for preparation of the "Glycyrrhizic Acid Reference Standard". The analytical data obtained were: UV spectrum: Lambda max, 251 nm; specific absorbance (E (1%) 1cm) in ethanol at 251 nm, 146; IR spectrum, specific absorptions at 1716,1656, 1215, and 1170 cm-1; and the spectrum of raw material was consistent with that of Standard (Control 941). Also, thin-layer chromatography, no impurities detected; high-performance liquid chromatography, three impurities detected. The amount of each impurity was estimated at less than 0.1%, and the total amount of impurities was less than 0.2%. Based on the above results, the candidate material was authorized as the Glycyrrhizic Acid Reference Standard (Control 991) of the National Institute of Health Sciences.
The concentrations of cocaine and benzoylecgonine (BE) in Standard Reference Material (SRM) 1508, cocaine and metabolites in freeze-dried human urine, were determined at the National Institute of Standards and Technology (NIST, formerly NBS) by two independent methods. For cocaine, one method was based on gas chromatography/mass spectrometry (GC/MS); the other was based on high-performance liquid chromatography (HPLC). For BE, one method was based on GC/MS; the other was based on flow injection analysis/thermospray mass spectrometry (FIA/MS). The results for each pair of methods were statistically evaluated. Concentrations were determined in the SRM for three levels of cocaine and three levels of benzoylecgonine. Methylecgonine, although present in the material, was not determined. For cocaine, the concentrations were 90, 263, and 429 ng/mL of human urine. For BE, the concentrations were 103, 259, and 510 ng/mL of human urine.