Liquid Chromatographic Determination of Vanillin and Related Aromatic Compounds

2000 ◽  
Vol 83 (1) ◽  
pp. 237-240 ◽  
Author(s):  
Eshwar Jagerdeo ◽  
Erin Passetti ◽  
Sumer M Dugar
Keyword(s):  
Aromatic Compounds ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Array Detector ◽  
Phase Measurements ◽  
Ethyl Vanillin ◽  
Photodiode Array Detector ◽  
Liquid Chromatographic

Abstract This paper describes a reversed-phase liquid chromatographic method for the determination of vanillin, associated natural aromatic compounds and/or synthetic precursors, ethyl vanillin, and coumarin, a commonly encountered adulterant in nonbeverage and beverage alcohol products using a ternary gradient mobile phase. The compounds were separated on a Nova-Pak C18 column by using water, methanol, and tetrahydrofuran as the mobile phase. Measurements were made by using a photodiode array detector at 275 nm. The choice of the mobile phase and the column provides baseline resolution of vanillin and the associated aromatic compounds commonly found in vanilla-flavoring material. Because this method provides low-level detection/quantitation, it is suitable for the characterization of vanilla flavoring materials that are currently added to vanilla flavored beverage alcohol products.

scholarly journals Liquid Chromatographic Determination of Sennosides in Cassia angustifolia Leaves

2006 ◽  
Vol 89 (4) ◽  
pp. 937-941 ◽  
Author(s):  
Alpana Srivastava ◽  
Richa Pandey ◽  
Ram K Verma ◽  
Madan M Gupta
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Sample Solution ◽  
Rapid Screening ◽  
Array Detector ◽  
Simple Liquid ◽  
Cassia Angustifolia ◽  
Photodiode Array Detector ◽  
Liquid Chromatographic

Abstract A simple liquid chromatographic method was developed for the determination of sennosides B and A in leaves of Cassia angustifolia. These compounds were extracted from leaves with a mixture of methanolwater (70 + 30, v/v) after defatting with hexane. Analyte separation and quantitation were achieved by gradient reversed-phase liquid chromatography and UV absorbance at 270 nm using a photodiode array detector. The method involves the use of an RP-18 Lichrocart reversed-phase column (5 μm, 125 × 4.0 mm id) and a binary gradient mobile-phase profile. The various other aspects of analysis, namely, peak purity, similarity, recovery, repeatability, and robustness, were validated. Average recoveries of 98.5 and 98.6%, with a coefficient of variation of 0.8 and 0.3%, were obtained by spiking sample solution with 3 different concentration solutions of standards (60, 100, and 200 μg/mL). Detection limits were 10 μg/mL for sennoside B and 35 μg/ML for sennoside A, present in the sample solution. The quantitation limits were 28 and 100 μg/mL. The analytical method was applied to a large number of senna leaf samples. The new method provides a reliable tool for rapid screening of C. angustifolia samples in large numbers, which is needed in breeding/genetic engineering and genetic mapping experiments.

scholarly journals Simultaneous Liquid Chromatographic Determination of Ezetimibe and Simvastatin in Pharmaceutical Products

2007 ◽  
Vol 90 (6) ◽  
pp. 1566-1572 ◽  
Author(s):  
Paulo Renato Oliveira ◽  
Thiago Barth ◽  
Vitor Todeschini ◽  
Sérgio luiz Dalmora
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Pharmaceutical Products ◽  
Array Detector ◽  
Control Analysis ◽  
Pharmaceutical Dosage Forms ◽  
Photodiode Array Detector ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic (LC) method was developed and validated for the simultaneous determination of ezetimibe and simvastatin in pharmaceutical dosage forms. The LC method was carried out on a Synergi fusion C18 column (150 mm 4.6 mm id) maintained at 45C. The mobile phase consisted of phosphate buffer 0.03 M, pH 4.5acetonitrile (35 + 65, v/v) run at a flow rate of 0.6 mL/min, and detection was made using a photodiode array detector at 234 nm. The chromatographic separation was obtained within 15.0 min, and calibration graphs were linear in the concentration range of 0.5200 g/mL. Validation parameters such as specificity, linearity, precision, accuracy, and robustness were evaluated, giving results within the acceptable range for both compounds. Moreover, the proposed method was successfully applied for the routine quality control analysis of pharmaceutical products.

scholarly journals Liquid Chromatographic Determination of Nitrofuran Residues in Bovine Muscle Tissues

1997 ◽  
Vol 80 (3) ◽  
pp. 481-485 ◽  
Author(s):  
Nora M Angelini ◽  
Oscar D Rampin ◽  
Héctor Mugica
Keyword(s):  
Mobile Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Uv Spectra ◽  
Array Detector ◽  
Bovine Muscle ◽  
Muscle Tissues ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method was developed and statistically validated for simultaneous determination of nitrofurazone, nitrofurantoin, furazolidone, and furaltadone residues in bovine muscle tissues. These antimicrobial residues in samples stabilized at pH 6.0 were extracted with acetonitrile and purified by liquid-liquid partition between dichloromethane-ethyl acetate and hexane saturated with acetonitrile. The acetonitrileethyl acetate extract was concentrated, and drug residues were dissolved in LC mobile phase, filtered, and determined by LC. A Cis reversed-phase (ODS Hypersil) column at 35°C, a mobile phase of 0.01 M sodium acetate buffer (pH 4.5)-acetonitrile (70 + 30), and a UV/visible diode array detector at 365 nm were used. The retention times and UV spectra of peaks in spiked samples were compared with those of known nitrofurans. Limits of detection (LD) and quantitation (LQ) were 1 and 2 μg/kg, respectively. Average recoveries were 76% (range, 60-110%). Relative standard deviations ranged from 6 to 18% at 5 fortification levels from 1.5 to 20 μg/kg. (Fortification levels for furaltadone were 3 to 40 μg/kg). The method was used to analyze 350 samples per year from 1993 to 1995.

Improved liquid-chromatographic determination of haloperidol in plasma.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).

Improved liquid-chromatographic determination of 3-methoxy-4-hydroxyphenylethyleneglycol in urine with electrochemical detection.

1984 ◽  
Vol 30 (1) ◽  
pp. 140-143 ◽  
Author(s):  
J R Shipe ◽  
J Savory ◽  
M R Wills
Keyword(s):  
Mobile Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Improved Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Mean Concentration ◽  
Phase Column

Abstract In this improved method for quantifying 3-methoxy-4-hydroxyphenylethyleneglycol (MHPG) in urine, after a multistep extraction of MHPG and internal standard (iso-MHPG) from 3.0 mL of urine, the compounds are separated on a C18 reversed-phase column and quantified by use of an electro-chemical detector. The isocratic chromatographic separation takes about 16 min. The mobile phase is phosphate buffer/acetonitrile (88/12 by vol), the flow rate 0.7 mL/min. Recycling the mobile phase and automating the sample injection make possible the unattended assay of more than 70 samples per day. The within-run precision of the method is excellent (CV 1.8%) at a mean concentration of 1.1 mg/L.

Liquid Chromatographic Determination of Vitamin D in Animal Feeds and Premixes

1992 ◽  
Vol 75 (5) ◽  
pp. 812-814 ◽  
Author(s):  
Vipin K Agarwal
Keyword(s):  
Vitamin D ◽  
Mobile Phase ◽  
Potassium Hydroxide ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Ultraviolet Detection ◽  
Animal Feeds ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method has been developed for the determination of vitamin D (D2 + D3) in animal feeds and premixes. The sample is saponified with potassium hydroxide, and vitamin D is extracted with hexane and isomerized to isotachysterol with 10M HCI in 2-butanol. LC determination of isotachysterol to quantitate vitamin D is carried out on a reversed-phase column with acetonitrilemethanol (90 +10) as the mobile phase and ultraviolet detection at 301 nm. The detection limit of the method is 1 lU/g. This method can also be used for the determination of vitamin D2 and D3 separately.

Liquid-chromatographic determination of pentobarbital in plasma with use of a resin column and an alkaline mobile phase.

1982 ◽  
Vol 28 (8) ◽  
pp. 1772-1774 ◽  
Author(s):  
R N Gupta ◽  
P T Smith ◽  
F Eng
Keyword(s):  
Mobile Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Enhanced Sensitivity ◽  
Acidic Drugs ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We describe a liquid-chromatographic method involving a new, nonsilica column (XAD-2, Hamilton Co.) for pentobarbital in plasma. Plasma is extracted with chloroform after addition of the internal standard, 5-ethyl-5-p-tolyl-barbituric acid. Acidic drugs are back-extracted into alkali, then chromatographed on the resin-base reversed-phase column. The use of alkaline mobile phase allows enhanced sensitivity and detection of barbiturates at 240 nm. The within-run CV for 10 samples was 1.9%, the between-run CV 1.8%. Ten commonly used barbiturates are separated isocratically in less than 15 min. Other commonly prescribed acidic drugs do not interfere with determination of pentobarbital.

scholarly journals Liquid Chromatographic Determination of Scopolamine, Hyoscyamine, and Phenobarbital in Tablets

1997 ◽  
Vol 80 (2) ◽  
pp. 331-334 ◽  
Author(s):  
Susan Ting
Keyword(s):  
Mobile Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Scopolamine Hydrobromide ◽  
Acid Sodium Salt ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method using a reversed- phase C18 column and octanesulfonic acid sodium salt-methanol as the mobile phase was developed for the simultaneous determination of phenobarbi- tal, scopolamine, and hyoscyamine in tablets. The mixture of the 3 drugs was resolved in <8 min. Detector responses were linear for 10 μL injections of the following: scopolamine hydrobromide, 8.25-206.3 μg/mL; hyoscyamine sulfate, 15.01-750.76 μg/mL; and phenobarbital, 250-751 μg/mL. Recoveries from tablets were 100.8% for scopolamine hydrobromide, 100.1% for hyoscyamine sulfate, and 100.3% for phenobarbital. Replicate injections of scopolamine hydrobromide, hyoscyamine sulfate, and phenobarbital gave an overall relative standard deviation of <1.0% (n = 10). The method detected as little as 3.3 ng scopolamine hydrobromide.

scholarly journals Liquid Chromatographic Determination of Histamine in Fish, Sauerkraut, and Wine: Interlaboratory Study

1998 ◽  
Vol 81 (5) ◽  
pp. 991-998 ◽  
Author(s):  
Paul R Beljaars ◽  
Remmelt Van Dijk ◽  
Klaas M Onker ◽  
Louis J Schout ◽  
◽  
...  
Keyword(s):  
Mobile Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Interlaboratory Study ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic ◽  
Postcolumn Derivatization

Abstract An interlaboratory study of the liquid chromatographic (LC) determination of histamine in fish, sauerkraut, and wine was conducted. Diminuted and homogenized samples were suspended in water followed by clarification of extracts with perchloric acid, filtration, and dilution with water. After LC separation on a reversed-phase C18 column with phosphate buffer (pH 3.0)-acetonitrile (875 + 125, v/v) as mobile phase, histamine was measured fluorometrically (excitation, 340 nm; emission, 455 nm) in samples and standards after postcolumn derivatization with ophthaldialdehyde (OPA). Fourteen samples (including 6 blind duplicates and 1 split level) containing histamine at about 10- 400 mg/kg or mg/L were analyzed singly according to the proposed procedure by 11 laboratories. Results from one participant were excluded from statistical analysis. For all samples analyzed, repeatability relative standard deviations varied from 2.1 to 5.6%, and reproducibility relative standard deviations ranged from 2.2 to 7.1%. Average recoveries of histamine for this concentration range varied from 94 to 100%

Liquid-chromatographic determination of alpha- and gamma-tocopherols in erythrocytes, with fluorescence detection.

1983 ◽  
Vol 29 (10) ◽  
pp. 1840-1842 ◽  
Author(s):  
J Lehmann ◽  
H L Martin
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We have adapted to erythrocytes a method for the determination of alpha- and gamma-tocopherols in plasma and platelets. Erythrocytes (50 microL) were extracted with methanol containing tocol (internal standard) and pyrogallol. Tocopherols were partitioned into chloroform, washed, and injected in methanol onto a reversed-phase (C18) "high-performance" liquid-chromatographic column. The mobile phase was methanol/water (99/1 by vol) at a flow rate of 2 mL/min and detection was with a "high-performance" spectrophotofluorometer. The limit of detection for either tocopherol is 0.10 microgram/mL of packed cells. Analytical recoveries ranged from 93 to 104%. Some values for tocopherols in human erythrocytes are presented.

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