Quantitative determination of titanium tetrachloride and dichloromethane by Raman spectroscopy using carbon disulfide as an internal standard

2020 ◽  
Vol 12 (7) ◽  
pp. 988-995
Author(s):  
Xiaoyan Xiang ◽  
Xianda He ◽  
Wentang Xia ◽  
Jianguo Yin ◽  
Xiaoli Yuan ◽  
...  

Raman spectroscopy with an internal standard and peak height ratio was applied for the quantitative analysis of dichloromethane and titanium tetrachloride.

2020 ◽  
pp. 13-16
Author(s):  
A. Y. Khrushchev ◽  
E. R. Akmaev ◽  
V. O. Bondarenko ◽  
A. E. Metlin

In this article we proposed a method for quantitative determination of active substance in pharmaceuticals via Raman scattering using potassium ferricyanide as internal standard. We approved this method in ketoprophenum quantitative determination in drug for veterinary use “Ketojekt”. The calculation of metrological requirements of procedures are established proposed method of calibration. Either we demonstrated the focalisation factor of laser beam affects on the method reproducibility. The method provides a precise, rapid, convenient to quantitative analysis that is more effective than the standard HPLC assay.


1980 ◽  
Vol 26 (1) ◽  
pp. 51-54
Author(s):  
D Jung ◽  
S Oie

Abstract We describe a simple, rapid chromatographic method for separating and quantitatively determining sulfisoxazole and its N4-acetyl metabolite in plasma and urine. A 100-micro L sample of plasma or urine is combined with 200 micro L of a solution containing 12 mg/L of the internal standard, N4-acetylsulfamethoxazole, in absolute methanol and centrifuged to obtain a clear supernatant solution. This solution is then eluted through a 10-micron microparticulate column with a mobile phase of 32/68 (by vol) methanol/sodium acetate buffer (0.01 mol/L, pH 4.7), at a flow rate of 1.2 mL/min. The eluted sompounds are detected by their absorption at 254 nm. We calculated concentration from the peak-height ratios of sulfisoxazole or N4-acetylsulfisoxazole to N4-acetylsulfamethoxazole. The peak-height ratio was linear with concentration in the range 0.05--200 mg/L for both drug and metabolite in plasma and urine. Because this assay can be completed within 30 min of obtaining a blood or urine sample, it should be a valuable tool in clinical drug monitoring and pharmacokinetic studies.


1983 ◽  
Vol 29 (12) ◽  
pp. 2100-2102 ◽  
Author(s):  
M Kelner ◽  
D N Bailey

Abstract We report a thin-layer-chromatographic micro-analysis for quinidine in serum, with detection by fluorescence densitometry. Quinidine is extracted from 20 microL of serum at pH 13 into 3 mL of hexane/acetone solution (80/20 by vol) containing N-(1-naphthyl)ethylenediamine as internal standard. The extract is concentrated and applied to silica-gel-impregnated plates for conventional thin-layer chromatography. Quinidine is identified from its RF value and quantified from the peak-height ratio between quinidine and the internal standard, relative to that of simultaneously extracted serum standards. The proposed assay is sensitive (to 0.2 mg/L), specific for unmetabolized quinidine, precise (between-run coefficients of variation less than 6%), and readily adaptable to large-scale "batch" analysis. Peak-height ratio is linearly related to concentration to at least 20 mg/L. Quinidine concentrations in the serum of patients, as measured by the proposed method (x) and by a traditional double-extraction spectrofluorometric assay (y), were related as follows: y = 0.994x + 0.276 (r = 0.989, n = 20).


2018 ◽  
Vol 5 (19) ◽  
pp. 22-28
Author(s):  
José Anchieta Gomes Neto ◽  
Silvana Ruella Oliveira ◽  
Felipe Fortunato ◽  
Marcos André Bechlin ◽  
Edilene Cristina Ferreira

1995 ◽  
Vol 50 (7) ◽  
pp. 624-630 ◽  
Author(s):  
M. A. Baker ◽  
J. Haupt ◽  
W. Gissler

For the determination of x and y of TiNx and TiBxNy coatings two Auger methods are presented, one circumventing and the other minimising the difficulties arising from the overlap of the KL23L23 and L3M23M23 peaks of N and Ti, respectively. The first method, developed for TiNx coatings, is based on the L3M23M45 valence band peak of Ti which develops a distinct second peak on nitridation, 3.9 eV below the main peak, labelled the L3M23Hybrid peak. After a simple Shirley background correction, a linear dependence of the L3M23Hybrid/L3M23M45 peak height ratio on the N/Ti ratio was found. This allows the determination of the N content of a TiNx compound. For TiBxNy coatings, a more complex shape of the L3M23M45 peak is obtained due to the presence of more than one phase, rendering this peak unusable for quantification. Therefore the N/Ti ratio is obtained from the L3M23M23/L3M23M4, peak intensity ratio for Ti. To minimise influences of the fine structure and improve the accuracy of the method, the negative peak excursions were artificially broadened. The N/Ti ratio so obtained is used in combination with the B concentration determined from the KL23L23 peak of B to yield the Ti-B-N composition.


2010 ◽  
Vol 7 (3) ◽  
pp. 751-756 ◽  
Author(s):  
Amit Gupta ◽  
Ram S. Gaud ◽  
S. Ganga

A simple and specific high performance thin layer chromatographic method was developed and validated for the determination of nisoldipine from tablet dosage form. The method was carried out at 320 nm after extraction of drug in methanol. The method uses aluminum plates pre-coated with silica gel 60F-254 as stationary phase and cyclohexane-ethyl acetate-toluene (3:3:4, v/v/v) as mobile phase. Linearity was established over a range of 400-2400 ng per zone. Both peak area ratio and peak height ratio showed acceptable correlation coefficienti.e.more than 0.99. However we used peak area for validation purpose. Intra-day and inter-day precision was determined and found to have less than 6.0 % RSD.


2015 ◽  
Vol 98 (3) ◽  
pp. 834-838 ◽  
Author(s):  
Pinggu Wu ◽  
Liqun Zhang ◽  
Xianghong Shen ◽  
Liyuan Wang ◽  
Yan Zou ◽  
...  

Abstract A sensitive and rapid analytical method based on alkaline diatomaceous earth extraction followed by GC/MS was developed for the quantitative determination of the toxic contaminant ethyl carbamate (EC) in yellow rice wines. The optimal extraction conditions were investigated. With the application of diatomaceous earth extraction, the damage of organic acids to the capillary column was greatly reduced. By using d5-EC as an internal standard for quantitative analysis of EC, the linearity of the calibration curves was good between 10 and 1000 ng/mL. The LOD and LOQ were 1.7 and 5.0 μg/kg, respectively. The spiked level of EC was 5.0–300 μg/kg, and the average recovery of the spikes was between 78.4 and 98.2%, with an RSD between 4.3 and 8.3%. Upon validation by five laboratories when spiked with 50, 100, and 300 μg/kg, the average respective recoveries were 102.9, 102.2, and 98.7% with a RSD between 0.7 and 8.1%. The validation results demonstrated that the method is fast, simple, selective, and suitable for the determination of EC in yellow rice wines.


1987 ◽  
Vol 33 (9) ◽  
pp. 1639-1642 ◽  
Author(s):  
K Oka ◽  
M Noguchi ◽  
T Kitamura ◽  
S Shima

Abstract We developed sensitive, specific "high-performance" liquid chromatography (HPLC) for determining suppressed cortisol and corticosterone in human plasma and compared its efficacy with that of conventional radioimmunoassay (RIA) at concentrations in the nanogram per liter range. Steroids from a 0.5-mL aliquot of plasma were extracted by rapid-flow fractionation, with diethyl ether as mobile-phase solvent, diatomaceous earth granules as stationary-support material. Analytical recovery of the steroids approached 100%. Concentrations in plasma were determined from peak-height ratio calibration (dexamethasone internal standard). The analytical column contained silica gel and the solvent system was water/methanol/dichloromethane/n-hexane (0.1/3/30/66.9 by vol). We could measure the steroids before and 20 h after oral administration of 0.5 mg of dexamethasone. The detection limit was 300 ng per liter of plasma for corticosterone, 500 ng/L for cortisol, with CVs of less than 4%. Determining corticosterone after administration of dexamethasone, in four of 20 such samples we could determine concentrations greater than 300 ng/L; the others contained corticosterone between 100 and 300 ng/L, but these values could not be certified analytically. Mean concentrations of these hormones as determined by RIA substantially exceeded those by HPLC. Some cross reactions in RIA could not be considered negligible in spite of pre-column treatment of the extracts.


1980 ◽  
Vol 26 (1) ◽  
pp. 51-54 ◽  
Author(s):  
D Jung ◽  
S Oie

Abstract We describe a simple, rapid chromatographic method for separating and quantitatively determining sulfisoxazole and its N4-acetyl metabolite in plasma and urine. A 100-micro L sample of plasma or urine is combined with 200 micro L of a solution containing 12 mg/L of the internal standard, N4-acetylsulfamethoxazole, in absolute methanol and centrifuged to obtain a clear supernatant solution. This solution is then eluted through a 10-micron microparticulate column with a mobile phase of 32/68 (by vol) methanol/sodium acetate buffer (0.01 mol/L, pH 4.7), at a flow rate of 1.2 mL/min. The eluted sompounds are detected by their absorption at 254 nm. We calculated concentration from the peak-height ratios of sulfisoxazole or N4-acetylsulfisoxazole to N4-acetylsulfamethoxazole. The peak-height ratio was linear with concentration in the range 0.05--200 mg/L for both drug and metabolite in plasma and urine. Because this assay can be completed within 30 min of obtaining a blood or urine sample, it should be a valuable tool in clinical drug monitoring and pharmacokinetic studies.


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