scholarly journals Multilinear Mathematical Separation in Chromatography

Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 31
Author(s):  
Yi Chen ◽  
Cong Ming Zou ◽  
Jun Bin ◽  
Min Yang ◽  
Chao Kang
Keyword(s):  
Chromatographic Separation ◽  
High Selectivity ◽  
Chemical Constituents ◽  
Internal Standard ◽  
Calibration Method ◽  
Complex Mixtures ◽  
Internal Standard Method ◽  
Elution Time ◽  
Standard Additions

Chromatography is a powerful and generally applicable method for the analytical separation and quantification of the chemical constituents in complex mixtures because chromatographic separation can provide high selectivity by isolating all analytes from interferences. Multiway analysis based on the multilinear model is an increasingly widely used method for interference-free and fast determination of the chemical constituents also in complex mixtures because multilinear mathematical separation can provide high selectivity by extracting the pure signal of the analyte from the mixed signal of a real sample. By combining chromatographic separation with mathematical separation, multiway calibration method, multiway standard additions method, and multiway internal standard method can be established. Chromatography assisted by multiway analysis can reduce the requirements for complete chromatographic separation, save elution time, and decrease the consumption of the mobile phase, particularly when the peak coelution problem is difficult to solve. This review presents the fundamentals and analytical applications of multilinear mathematical separation in chromatography.

Determination of alcohols in mixtures by 19F NMR spectroscopy using hexefluoroacetone reagent

1982 ◽  
Vol 47 (7) ◽  
pp. 1973-1978 ◽  
Author(s):  
Jiří Karhan ◽  
Zbyněk Ksandr ◽  
Jiřina Vlková ◽  
Věra Špatná
Keyword(s):  
Standard Deviation ◽  
Nmr Spectroscopy ◽  
Standard Method ◽  
Internal Standard ◽  
Internal Standard Method ◽  
Concentration Region ◽  
Experimental Conditions ◽  
Curve Method ◽  
Sample Preparation Procedure

The determination of alcohols by 19F NMR spectroscopy making use of their reaction with hexafluoroacetone giving rise to hemiacetals was studied on butanols. The calibration curve method and the internal standard method were used and the results were mutually compared. The effects of some experimental conditions, viz. the sample preparation procedure, concentration, spectrometer setting, and electronic integration, were investigated; the conditions, particularly the concentrations, proved to have a statistically significant effect on the results of determination. For the internal standard method, the standard deviation was 0.061 in the concentration region 0.032-0.74 mol l-1. The method was applied to a determination of alcohols in the distillation residue from an oxo synthesis.

Measurement of sodium valproate in serum by direct-insertion chemical-ionization/mass spectrometry.

1980 ◽  
Vol 26 (1) ◽  
pp. 147-149
Author(s):  
G M Schier ◽  
I E Gan ◽  
B Halpern ◽  
J Korth
Keyword(s):  
Mass Spectrometry ◽  
Stable Isotope ◽  
Sodium Valproate ◽  
Chromatographic Separation ◽  
Chemical Ionization ◽  
Internal Standard ◽  
Ionization Mass Spectrometry ◽  
Chemical Ionization Mass Spectrometry ◽  
Ionization Mass

Abstract To quantitatively determine sodium valproate, we use a stable isotope-labeled internal standard and chemical-ionization/mass spectrometry, without prior chromatographic separation. The technique is rapid, simple, sensitive, and provides for the routine analysis of 100 microL of serum with good within-day and day-to-day precision. The technique also allows for the simultaneous determination of phenobarbital, mephobarbital, carbamazepine, primidone, and phenytoin.

Regulatory Approach to Determination of Lysine in Feedstuffs by Liquid Chromatography with Fluorescence Detection via Precolumn Dansylation

1989 ◽  
Vol 72 (4) ◽  
pp. 609-613 ◽  
Author(s):  
Alan Thio ◽  
David H Tompkins
Keyword(s):  
Liquid Chromatography ◽  
Animal Feed ◽  
Internal Standard ◽  
Internal Standard Method ◽  
Fluorescence Detector ◽  
The Matrix ◽  
Regulatory Approach ◽  
Small Aliquot ◽  
Calculated Amount

Abstract A method for compliance analysis for total lysine in animal feed is described. One g portions of finely ground feed sample are spiked with a calculated amount of diaminobutyric acid internal standard and hydrolyzed by heating with 100 mL 6N aqueous HC1 at 120°C in a closed bottle. A very small aliquot (25 /*L) of hexane-washed hydrolysate is evaporated under vacuum to dryness and derivatized with dansyl chloride. Lysine is separated from other amino acids by isocratic reverse-phase (LC-18) liquid chromatography; the mobile phase is acetonitrile-O.OlM sodium phosphate (pH 7.0) buffer (100 + 210, v/v). The internal standard method along with a fluorescence detector (310-410 nm excitation and 435-650 nm emission), is used for quantitation. Thirty-five feed samples of various types (lysine 0.2- 8.2%) were analyzed with no interference from the matrix. The results were compared with those furnished by an independent laboratory using an amino acid analyzer; no statistical difference was found at the 95% confidence level. Six replicate analyses of a feed sample showed a coefficient of variation of 2.8%; no significant differences were found when between-day results of 9 samples (lysine 0.90- 4.30%) were compared. This procedure has been tested for ruggedness and can be applied for compliance determination of total lysine in feedstuffs by laboratories with limited resources

Determination of retinol, alpha-tocopherol, and beta-carotene in serum by liquid chromatography with absorbance and electrochemical detection.

1987 ◽  
Vol 33 (9) ◽  
pp. 1585-1592 ◽  
Author(s):  
W A MacCrehan ◽  
E Schönberger
Keyword(s):  
Electrochemical Detection ◽  
Chromatographic Separation ◽  
Protein Denaturation ◽  
Internal Standard ◽  
Beta Carotene ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Alpha Tocopherol ◽  
Phase Gradient

Abstract We describe a method for the determination of retinol, alpha-tocopherol, and beta-carotene in serum, using a liquid-chromatographic separation with wavelength-programmed ultraviolet/visible absorbance and amperometric electrochemical detection with a glassy carbon electrode. After protein denaturation and addition of an internal standard, tocol, 250-microL samples are twice extracted with hexane. The reversed-phase, gradient-elution chromatographic separation provides baseline resolution of: the all-trans isomer of retinol from the cis isomers, alpha- from gamma-tocopherol, and all-trans-beta-carotene from alpha-carotene and from cis-beta-carotene isomers. The linearity of response and the detection limits for the two detectors for the three analytes are measured. A comparison of the values obtained for serum extracts shows good agreement between the absorbance and electrochemical detectors.

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