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At least 19 recordsLinked to original sources

Comparison of the determination of magnesium by methylthymol blue spectrophotometry and atomic absorption spectrophotometry.

Plasma samples (n = 155) of 30 patients on an intensive ward were analysed for magnesium simultaneously by atomic absorption spectrophotometry (AAS) and methylthymol blue spectrophotometry. Methylthymol blue spectrophotometry was performed at the bedside, using two different multianalysers, Easy ST 1 and Easy ST 2, Merck, D-Darmstadt. Precision was 12.2% (Easy ST 1) and 17.1% (Easy ST 2), and the average value was 0.89 mmol/l, which was above the expected range (0.72-0.88 mmol/l). Accuracy was 16.25% (Easy ST 1) and 8.75% (Easy ST 2). Analyser 2 was more accurate (8.75% versus 6.25%) but less precise (17.1% versus 12.2%) than analyser 1. Precision of AAS was between the expected values of 0.69 and 0.84 mmol/l. Easy ST and AAS gave significantly different values (p < 0.0001) for 155 measurements. Comparison of AAS and methylthymol blue spectrophotometery showed that methylthymol blue spectrophotometry produced higher values than AAS (mean difference 0.186 mmol/l). Furthermore, analyses of 40 samples of a standardized plasma concentration with methylthymol blue spectrophotometry showed a very low precision (15.3%). Easy ST cannot be assigned for urinary measurements of magnesium. Experimentally measured samples gave unaccountable results.

Bromthymol Blue↗

Advantage of zero-crossing-point first-derivative spectrophotometry for the quantification of calcium oxalate crystalline phases by infrared spectrophotometry.

The main component of urinary calculi in industrialized countries is calcium oxalate. Its detection in stones is easily performed by infrared spectrophotometry. However its two crystalline forms calcium oxalate monohydrate (COM) and calcium oxalate dihydrate (COD), which are linked to different aetiologies, provide similar patterns, with overlapping vibrations leading to difficulties in differentiation and quantitation of both the phases in mixtures. Some minor but characteristic bands of each crystalline species are emphasized for analytical purposes. The method of zero-crossing-point first-derivative spectrophotometry was applied to calcium oxalate species quantitation and revealed to be easy, accurate, precise and very well adapted to routine laboratories.

Calcium Oxalate↗

Comparative sensitivities of flame atomic absorption spectrophotometry (AAS) and molecular absorption spectrophotometry (MAS).

A sensitivity comparison was made between conventional atomic absorption spectrophotometry (AAS) and conventional molecular absorption spectrophotometry (MAS) for the serum trace metals, copper, iron, and zinc. The sensitivity aspect considered was absorbances was obtained for concentrations in the solutions analyzed using unit lightpaths of 1 cm and 10 cm for MAS and AAS, respectively. A distinction was made between procedural sensitivity and measurement sensitivity where the latter represents molar absorptivity. Some was given to the concepts of procedural sensitization by concentration of the analyte through the use of lyophilization, extraction or ashing. The misuse of data obtained with scale expanders is described as a commonly occurring phenomenon of both AAS and MAS and a source of confusion in the understanding of measurement sensitivity.

Copper↗

Application of TLC-densitometry, first-derivative UV-spectrophotometry and ratio derivative spectrophotometry for the determination of dorzolamide hydrochloride and timolol maleate.

Three methods are described for the simultaneous determination of dorzolamide hydrochloride (DORZ) and timolol maleate (TIM) in ophthalmic solutions. The first method is based on application of thin layer chromatographic separation of both drugs followed by the densitometric measurements of their spot areas. After separation on silica gel GF(254) plates, using methanol-ammonia 25% (100:1.5 v/v) as the mobile phase, the chromatographic zones corresponding to the spots were scanned at 253 and 297 nm, respectively. The calibration function was established in the ranges of 2-18 microg for DORZ and 0.5-4.5 microg for TIM. The second method depends on first derivative ultraviolet spectrophotometry, with zero-crossing measurement method. The first derivative values D(1) at 250.2 and 312.5 nm were selected for the assay of DORZ and TIM, respectively. Calibration graphs follow Beer's law in the range 10-64 and 2.5-16 microg ml(-1), respectively. The third method is based on ratio first derivative spectrophotometry. The signals in the first derivative of the ratio spectra at 244 and 306.2 nm were selected to determine DORZ and TIM in the mixture and calibration graphs are linear in the range of 5-40 and 5.0-17.5 microg ml(-1), respectively. The proposed methods were successfully applied to the determination of these compounds in synthetic mixtures and in pharmaceutical preparations. The proposed methods are simple, rapid and suitable for quality control application.

Antihypertensive Agents↗

Comparison of direct (X-ray diffraction and infrared spectrophotometry) and indirect (infrared spectrophotometry) methods for the analysis of alpha-quartz in airborne dusts.

In this study, the alpha-quartz contents measured by different analytical techniques (X-ray diffraction, direct method; and infrared spectrophotometry, direct and indirect methods) were compared. The analyses were carried out on filters sampled in an industrial setting by means of a Dorr-Oliver cyclone. To verify the methodology used, filters loaded with pure alpha-quartz were also analysed. By and large, the agreement between the two direct methods was close on average, but on the basis of a comparison of the individual results, considerable differences exist. In absolute value, the mean relative deviation between the two techniques was <25% in only 47.8% of the cases. The results obtained by the indirect method (infrared) were on average 13% lower than the results obtained by the two direct methods with a more important difference (23%) for samples where calcite was identified by X-ray diffraction in comparison with those where it was not (8%). This underestimation, which was not owing to dust losses during preparation, is probably explained by the elimination of organic compounds during dust calcinations or by the transformation of mineral compounds. The indirect method introduces additional sample handling operations with more risk of material loss. When the quantity of calcined material was <0.4 mg, the weighing operations necessary to correct any losses of material resulted in considerable variability. In terms of overall uncertainty, it would be better in this case not to carry out correction and to employ an operating mode favouring the recovery of a maximum of material while accepting a bias of about 5-7%.

Air Pollutants↗

Application of first derivative UV-spectrophotometry and ratio derivative spectrophotometry for the simultaneous determination of candesartan cilexetil and hydrochlorothiazide.

Two-component mixtures of candesartan cilexetil (CAN) and hydrochlorothiazide (HYD) were assayed by first derivative and ratio derivative spectrophotometry. The first method depends on zero-crossing and peak to base measurement. The first derivative amplitudes at 270.1 and 255.5 nm were selected for the assay of (CAN) and (HYD), respectively. The second method depends on first derivative of the ratio spectra by division of the absorption spectrum of the binary mixture by a normalized spectrum of one of the components and then calculating the first derivative of the ratio spectrum. The first derivative of the ratio amplitudes at 236, 250, 232, 267 and 280 nm were selected for the determination of (CAN) and (HYD), respectively. Calibration curves were established for 6.0-38.0 microg x ml(-1) for (CAN) and 4.0-28.0 microg x ml(-1) for (HYD) in binary mixtures. Good linearity, precision and selectivity were found, and the two methods were successfully applied to the pharmaceutical dosage form containing the above-mentioned drug combination without any interference by the excipients.

Antihypertensive Agents↗

Determination of chlorprothixene and amitryptyline hydrochlorides by UV-derivative spectrophotometry and UV-solid-phase spectrophotometry.

Two methods for spectrophotometric determination of chlorprothixene and amitryptyline hydrochlorides were proposed. One of them is based on spectral analysis of their derivative spectra. The measurement of the value at 316.0 nm of first derivative was used for construction of calibration graph for chlorprothixene. The Beer law was obeyed in the concentration range 0.5-50.0 microg ml(-1). The amplitude of the second derivative at 261.4 nm was used for determination of amitryptyline in the range 0.5-75.0 microg ml(-1). The second proposed method is utilized the use of solid sorbent for simultaneous preconcentration and assay of studied compounds. For this purpose the filtration gel Sephadex G100 was applied. The elaborated solid-phase spectrophotometric method was used for determination of chlorprothixene at 268.0 nm in the range 2.5-75.0 microg ml(-1) and amitryptyline at 238.0 nm in the concentration range 10.0-75.0 microg ml(-1).

Amitriptyline↗

Determination of phenolphthalein and methylene blue by first derivative spectrophotometry and potassium nitrate by direct spectrophotometry in a pharmaceutical formulation.

A rapid first derivative visible spectrophotometric determination is described for the simultaneous determination of phenolphthalein (PHP) and methylene blue (MB) in the presence of potassium nitrate (KNO3). Potassium nitrate is also determined by direct visible spectrophotometric method in the presence of phenolphthalein and methylene blue without any interference. The methods have been applied to the determination of the three compounds in a commercial dosage form. The calibration graphs were linear in the range of 0.30-3.20 mg mL-1 for MB and 0.80-3.18 micrograms mL-1 for PHP and 0.80-8.10 micrograms mL1 for KNO3. The specificity, accuracy and precision of the methods have been assessed.

Calibration↗

Determination of trans unsaturation by infrared spectrophotometry and determination of fatty acid composition of partially hydrogenated vegetable oils and animal fats by gas chromatography/infrared spectrophotometry: collaborative study.

An infrared spectrophotometric (IR) method for the determination of total trans unsaturated fatty acid (trans) content and a combined gas-liquid chromatographic/infrared spectrophotometric (GC/IR) method for determination of fatty acid composition of partially hydrogenated vegetable oils (PHVO) were studied collaboratively in 12 laboratories using 7 PHVO samples, including 1 pair of blind duplicates. The test samples were methylated and analyzed for total trans content by IR and for fatty acid composition by GC/IR using a capillary column coated with SP-2560 or another suitable cyanoalkylsiloxane stationary phase. From the measured IR absorption, the isolated trans content was calculated using a calibration curve of absorption versus trans content developed with 2-component calibration standard mixtures of methyl elaidate and oleate. The GC provided the levels of mono-trans-octadecadienoates (18:2t), di-trans-octadecadienoates (18:2tt) and mono-trans-octadecatrienoates (18:3t). The trans-octadecenoate (18:1t) content was calculated with the formula: 18:1t = IR trans-0.84 x (18:2t + 18:3t) - 1.74 x 18:2tt. The cis-octadecenoate (18:1c) content was obtained as the difference between total octadecenoates (18:1) and 18:1t. Reproducibility relative standard deviations (RSDR) for 15 to 35% trans content determined by IR were in the range of 8.8-11.7%, whereas RSDR for the test sample with 5% trans content was 34.6%. RSDR values for 18:1t by the GC/IR followed the same pattern as that of IR trans values: 36.4% for the test sample with 4.9% 18:1t versus 7.8-12.5% for test samples with 14.9 to 32.6% 18:1t. The content of 18:1c in the test samples varied from 24.7 to 34.5% and their RSDR values ranged from 3.8 to 10.5%. The mean values for 18:1t and 18:1c compared favorably with the absolute levels determined by a silver nitrate-thin layer chromatography/GC procedure. The IR and GC/IR methods are recommended for determination of trans content and fatty acid composition, respectively, of partially hydrogenated fats derived from vegetable oils, terrestrial animal fats or such oils and fats isolated from food products containing > 5% trans fatty acids. For samples containing < or = 5% trans fatty acids, a direct GC method (American Oil Chemists' Society Official Method Ce 1c-89) is available for determination of both trans content and fatty acid composition, because at lower trans levels, overlap of 18:1 cis and trans isomers on GC with very polar capillary columns is negligible.(ABSTRACT TRUNCATED AT 400 WORDS)

Chromatography, Gas↗

Determination of hepatic tissue calcium levels by flame emission spectrophotometry.

Hepatotoxicants are known to cause significant increases in total liver calcium content. These increases are postulated to be the key irreversible event leading to necrosis of hepatic parenchymal cells. An investigation is presented of the use of flame emission spectrophotometry as an alternative analytical method to atomic absorption spectrophotometry in the assessment of hepatic calcium levels following hepatotoxicant challenge, using a proven method of tissue digestion. Flame emission and atomic absorption spectrophotometry were found to be comparable in sensitivity with detection limits in the ppm range and correlation coefficients of greater than 0.99 for the standard curves. Tissue sample analysis demonstrated comparable precision for the two methods. The liver calcium levels determined for an untreated control rat were 105 ppm with a coefficient of variation of 2.9% for flame emission spectrophotometry vs. 106 ppm with a coefficient of variation of 3.6% for atomic absorption spectrophotometry. Comparable precision was also found for the two methods when toxicant-damaged liver was analyzed. Flame emission spectrophotometry appears to be a useful alternative to atomic absorption spectrophotometry for tissue calcium analyses in experimental toxicologic studies.

Animals↗

Plasma elimination of indocyanine green in the intact pig after bolus injection and during constant infusion: comparison of spectrophotometry and high-pressure liquid chromatography for concentration analysis.

Indocyanine green is used to estimate liver blood flow rate and hepatic intrinsic clearance. However, its use as a test substance for studies of liver function has been limited by two puzzling kinetic observations: a biexponential plasma decay after bolus injection with an extremely slow late phase and an apparently steadily decreasing clearance value during constant infusion. These observations have been made with spectrophotometric concentration analysis. In anesthetized 30- to 40-kg pigs, we examined plasma concentration curves of indocyanine green after intravenous bolus injection and during long-term infusion. We compared spectrophotometry with high-pressure liquid chromatography for measurement of plasma indocyanine green concentration. In freshly prepared commercially available indocyanine green, high-pressure liquid chromatography could separately measure two fractions, the genuine indocyanine green (97% to 99% of total) and an in vitro degradation product (1% to 3%). Because their spectra were nearly identical, these fractions could not be distinguished by spectrophotometry. After intravenous administration both fractions were identified in the plasma by high-pressure liquid chromatography. In the first series (n = 6) 25 mg of indocyanine green was injected intravenously for 5 min. When analyzed by high-pressure liquid chromatography, the genuine indocyanine green plasma concentration decay was biexponential with rate constants 0.196 +/- 0.021 (mean +/- S.E.M., n = 6) and 0.0372 +/- 0.0064 min-1. The degradation product of indocyanine green decayed almost monoexponentially, with a rate constant of 0.0093 +/- 0.0002 min-1. With spectrophotometry a biexponential decay was observed with rate constants 0.130 +/- 0.012 and 0.0095 +/- 0.0001 min-1. The biexponential decay of indocyanine green after spectrophotometry was the result of codetermination of the two fractions: genuine indocyanine green was responsible for initial phase, and the degradation product of indocyanine green was responsible for the late phase. In the second series (n = 9), indocyanine green was administered as a constant intravenous infusion. From 90 to 240 min the intrinsic hepatic clearance of genuine indocyanine green did not change detectably with time. In contrast, the degradation product of indocyanine green never reached steady-state concentrations. Because of code-termination of these two indocyanine green fractions, the apparent intrinsic hepatic clearance of indocyanine green estimated from spectrophotometry was steadily decreasing by 8.9% +/- 1% per hour of its initial value. At the same time estimation of liver plasma flow rate based on Fick's principle was not affected by the choice of analytical methodology. These observations indicate that high-pressure liquid chromatography is superior to spectrophotometry for kinetic analysis of indocyanine green elimination.

Animals↗

CSF spectrophotometry in the diagnosis and exclusion of spontaneous subarachnoid haemorrhage.

AIMS: To assess the sensitivity and specificity of CSF spectrophotometry for the detection of xanthochromia in patients with clinical symptoms suggestive of subarachnoid haemorrhage (SAH) but normal cranial computed tomography (CT). METHODS: All consecutive patients undergoing both cranial CT and lumbar puncture for investigation of possible SAH at the Princess Alexandra Hospital, Brisbane, between January 2000 and April 2003 were included in the study. All case histories, radiology and laboratory results were retrospectively assessed. The sensitivity, specificity and positive predictive value of the spectrophotometry test were calculated. RESULTS: 253 patients were included in the study. Spectrophotometry was shown to have a sensitivity of 100% but a specificity of only 75.2%. The positive predictive value of spectrophotometry as an indicator of SAH was 3.3%. CONCLUSIONS: CSF spectrophotometry has an unacceptably low specificity and positive predictive value, which greatly limit its use as a clinical tool.

False Positive Reactions↗

Is cerebrospinal fluid spectrophotometry useful in CT scan-negative suspected subarachnoid haemorrage?

Missed cerebral aneurysms in CT-negative patients can have serious implications. We set out to determine the usefulness of cerebrospinal fluid (CSF) spectrophotometry and the individual significance of CSF oxyhaemoglobin, bilirubin and methaemoglobin in 463 CT scan-negative patients with suspected subarachnoid haemorrhage (SAH) and normal neurological examination. CSF spectrophotometry resulted in the diagnosis of an intracranial aneurysm in 2% (9/463) of patients with CT-negative suspected SAH. No aneurysms were found in patients in whom spectrophotometry was negative for haem pigments. Less than 1% of patients with oxyhaemoglobin alone had aneurysms diagnosed, whilst 21% of patients with bilirubin had an aneurysm. CSF spectrophotometry is an important investigation in patients with CT-negative suspected SAH, particularly where clinical suspicion is strong. Patients positive for bilirubin are likely to provide a high yield of aneurysmal bleed and should undergo angiography. Patients with oxyhaemoglobin alone in whom SAH is strongly suspected may benefit from angiography. Based on a small number of patients, we recommend that patients with methaemoglobin should also be investigated. Patients with negative spectrophotometry are unlikely to benefit from further investigation.

Bilirubin↗