Determination of Acesulfam-K in Foods

1993 ◽  
Vol 76 (2) ◽  
pp. 268-274 ◽  
Author(s):  
Jacques Prodolliet ◽  
Milene Bruelhart
Keyword(s):  
Fruit Juice ◽  
Soft Drink ◽  
Food Additives ◽  
Reversed Phase ◽  
Uv Absorbance ◽  
Phase Detection ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method was evaluated for the determination of the intense sweetener acesulfam-K in tabletop sweetener, candy, soft drink, fruit juice, fruit nectar, yogurt, cream, custard, chocolate, and biscuit commercial preparations. Samples are extracted or simply diluted with water and filtered. Complex matrixes need a clarification step with Carrez solutions. An aliquot of the extract is analyzed on a reversed-phase μBondapak C18 column using 0.0125M KH2PO4 (pH 3.5)-acetonitrile (90 + 10) as mobile phase. Detection is performed by UV absorbance at 220 nm. Recoveries ranged from 95.2 to 106.8%. With one exception, all analyzed values were within ±15% of the declared levels. The repeatabilities and the repeatability coefficients of variation were, respectively, 0.37 mg/100 g and 0.98% for products containing less than 40 mg/100 g acesulfam-K and 2.43 mg/100 g and 1.29% for other products. The same procedure also allowed detection of many food additives or natural constituents, such as other intense sweeteners, organic acids, and alkaloids, in a single run without interfering with acesulfam-K. The method is simple, rapid, precise, and sensitive; therefore, it is suitable for routine analyses.

Determination of Aspartame and Its Major Decomposition Products in Foods

1993 ◽  
Vol 76 (2) ◽  
pp. 275-282 ◽  
Author(s):  
Jacques Prodolliet ◽  
Milene Bruelhart
Keyword(s):  
Soft Drink ◽  
Food Additives ◽  
Reversed Phase ◽  
Food Samples ◽  
Phase Detection ◽  
Decomposition Products ◽  
Coefficients Of Variation ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract A liquid chromatographic procedure already evaluated in a preceding study for the analysis of acesulfam-K is also suitable for the determination of the intense sweetener aspartame in tabletop sweetener, candy, fruit beverage, fruit pulp, soft drink, yogurt, cream, cheese, and chocolate preparations. The method also allows the determination of aspartame’s major decomposition products: diketopiperazine, aspartylphenylalanine, and phenylalanine. Samples are extracted or diluted with water and filtered. Complex matrixes are centrifuged or clarified with Carrez solutions. An aliquot of the extract is analyzed on a reversed-phase μBondapak C18 column using 0.0125M KH2P04 (pH 3.5)-acetonitrile ([85 + 15] or [98 + 2]) as mobile phase. Detection is performed by UV absorbance at 214 nm. Recoveries ranged from 96.1 to 105.0%. Decomposition of the sweetener was observed in most food samples. However, the total aspartame values (measured aspartame + breakdown products) were within -10% and +5% of the declared levels. The repeatabilities and the repeatability coefficients of variation were, respectively, 1.00 mg/100 g and 1.34% for products containing less than 45 mg/100 g aspartame and 4.11 mg/100 g and 0.91 % for other products. The technique is precise and sensitive. It enables the detection of many food additives or natural constituents, such as other intense sweeteners, organic acids, and alkaloids, in the same run without interfering with aspartame or its decomposition products. The method is consequently suitable for quality control or monitoring.

Improved liquid-chromatographic method for determination of serum cortisol.

1979 ◽  
Vol 25 (7) ◽  
pp. 1293-1296 ◽  
Author(s):  
P M Kabra ◽  
L L Tsai ◽  
L J Marton
Keyword(s):  
Limit Of Detection ◽  
Internal Standard ◽  
Serum Cortisol ◽  
Peak Height ◽  
Reversed Phase ◽  
Column Temperature ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract We describe a specific and precise method for measuring concentrations of cortisol in serum or plasma by liquid chromatography. Cortisol, together with an internal standard, equilenin, is extracted from 1 mL of serum or plasma and analyzed isocratically on a reversed-phase column with a mobile phase of acetonitrile/phosphate buffer (30/70, by vol.), at a flow rate of 2.0 mL/min. The eluted cortisol is detected by its absorption at 254 nm and quantitated by peak height measurements. Each analysis requires no longer than 15 min at the optimum column temperature of 50 degrees C. The lower limit of detection for cortisol is about 2 ng/sample for a standard solution; sensitivity is routinely 5 micrograms/L of serum. Analytical recoveries exceeded 95%, with good day-to-day precision (coefficients of variation between 4 and 7%). Of more than 50 drugs and steroids tested for possible interference, only the steroids cortisone, prednisone, and prednisolone may interfere with the analysis of cortisol.

Liquid Chromatographic Determination of Saccharin in Beverages and Sweets: NMKL Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 58-60 ◽  
Author(s):  
Anna-Maija K Sjoberg ◽  
Timo A Alanko
Keyword(s):  
Chromatographic Method ◽  
Soft Drink ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Sodium Saccharin ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A reverse phase liquid chromatographic method for the determination of saccharin in a soft drink and a juice was collaboratively studied in 8 laboratories. Collaborators were supplied with 3 samples of the soft drink and 3 samples of the juice containing sodium saccharin levels of 40-100 mg/L. Average recoveries of sodium saccharin were 95.3% for the soft drink and 98.0% for the juice. The reproducibility coefficients of variation were 16.9% for the soft drink and 10.4% for the juice. In addition, a mini-collaborative study was conducted for the determination of saccharin in 3 samples of sweets produced commercially. Five collaborators analyzed the samples, which contained saccharin at levels of 100-600 mg/kg according to the maker's specifications. Saccharin was extracted with water and ethanol and chromatographed using a modified liquid chromatographic method. The reproducibility coefficient of variation was 12.4% for the sweets.

scholarly journals Application of Liquid Chromatography to the Simultaneous Determination of Acetylsalicylic Acid, Caffeine, Codeine, Paracetamol, Pyridoxine, and Thiamine in Pharmaceutical Preparations

2001 ◽  
Vol 84 (3) ◽  
pp. 676-683 ◽  
Author(s):  
Natividad Ramos-Martos ◽  
Francisco Aguirre-Gómez ◽  
Antonio Molina-Díaz ◽  
Luis F Capitán-Vallvey
Keyword(s):  
Salicylic Acid ◽  
Acetylsalicylic Acid ◽  
Simultaneous Determination ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract This paper describes a rapid reversed-phase liquid chromatographic method, with UV detection, for the simultaneous determination of acetylsalicylic acid, caffeine, codeine, paracetamol, pyridoxine, and thiamine in pharmaceutical preparations. A reversed-phase C18 Nucleosil column is used. The mobile phase consists of 2 successive eluants: water (5 min) and acetonitrile–water (75 + 25, v/v; 9 min), both adjusted to pH 2.1 with phosphoric acid. Before determination acetylsalicylic acid is completely converted to salicylic acid by alkaline hydrolysis. Salicylic acid, caffeine, paracetamol, pyridoxine, and thiamine are all detected at 285 nm, whereas codeine is detected at 240 nm. Calibration curves were linear for salicylic acid, caffeine, paracetamol, and pyridoxine in the range of 50–500 mg/L, and for codeine and thiamine in the range of 50–1000 mg/L. The method was applied to the analysis of 13 fortified commercial pharmaceutical preparations. Recoveries ranged from 92.6 to 105.5%, with relative standard deviations of 1.1–5.8%.

Optimized liquid-chromatographic determination of metronidazole and its metabolites in plasma.

1984 ◽  
Vol 30 (5) ◽  
pp. 784-787 ◽  
Author(s):  
R A Gibson ◽  
L Lattanzio ◽  
H McGee
Keyword(s):  
Rapid Determination ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Detector Response ◽  
High Pressure Liquid Chromatographic ◽  
Liquid Chromatographic Method ◽  
Wide Range ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Metronidazole and its known metabolites in plasma can be rapidly separated by a "high-pressure" liquid-chromatographic method that can also be adapted for rapid determination of tinidazole. Samples deproteinized with trichloroacetic acid (50 g/L final concentration) undergo isocratic separation on a reversed-phase C18 column eluted with an 8/92 (by vol) mixture of acetonitrile/KH2PO4 (5 mmol/L, pH 3.0). The method is sensitive, reliably detecting as little as 25 micrograms of metronidazole and (or) its metabolites per milliliter of plasma. The detector response varied linearly with concentration for all compounds tested over a wide range (25-500 micrograms/L). Within-day and between-day variation was generally less than 2.5% for all concentrations of all compounds tested. Various other antibiotics tested did not interfere.

DEVELOPMENT AND VALIDATION OF A NEW RP HPLC METHOD FOR ROUTINE DETERMINATION OF TEA TREE OIL IN BULK AND COSMECEUTICAL FORMULATIONS

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 43-49
Author(s):  
B.P. Manjula ◽  
V. G Joshi ◽  
Siddamsetty Ramachandra Setty ◽  
M Geetha ◽  
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Tea Tree Oil ◽  
Tea Tree ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

Tea tree oil, an active ingredient of skin, hair and nail care cosmeceuticals, has claims for topical antimicrobial, analgesic and anti-inflammatory activity. Its complex composition is governed by ISO 4730:2017. Terpinene-4-ol is the principal constituent of the oil (35% - 48%) followed by γ-terpinene (14% -28%), α-terpinene (6%-12%) and 1,8-cineole (≤15%). A reversed-phase, isocratic high performance liquid chromatographic method has been developed and validated for routine determination of tea tree oil based on1,8-cineole content in bulk and commercially available cosmeceuticals using C18 column, methanol-water (70:30 v/v) as mobile phase and flow rate of 1mL/min. UV detection was done at 200 nm. Linearity of the method was established for 20-100μL/mL (R2 = 0.9992) with LOD, LOQ values of 0.5594 μL/mL and 5.5941μL/mL respectively. The % RSD values for robustness and precision were <1% and recovery ranged between 99.09-102.96%. The method was successfully applied for determination of 1,8-cineole content in cosmeceuticals.

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