Reverse Phase Liquid Chromatographic Determination of Some Food Additives

1987 ◽  
Vol 70 (3) ◽  
pp. 578-582 ◽  
Author(s):  
Madduri Veerabhadrarao ◽  
Mandayam S Narayan ◽  
Omprakash Kapur ◽  
Chilukuri Suryaprakasa Sastry
Keyword(s):  
Acetic Acid ◽  
Benzoic Acid ◽  
Mobile Phase ◽  
Direct Method ◽  
Food Additives ◽  
Acid Water ◽  
Relative Standard ◽  
Acetic Acid Water ◽  
Liquid Chromatographic

Abstract Liquid chromatographic methods are described for the separation and determination of non-nutritive sweeteners, namely, acesulfame, aspartame, saccharin, and dulcin; preservatives such as benzoic acid and p-hydroxybenzoic acid; and caffeine and vanillin in ready-toserve beverages, ice candy, ice cream, squash beverage, tomato sauce, and dry beverage mix samples. These additives are separated on a ^Bondapak C18 column using methanol-acetic acid-water (20 + 5 + 75) as mobile phase and detected by UV absorption at 254 nm. Caffeine, vanillin, dulcin, and benzoic acid can be analyzed quickly by using a mobile phase of methanol-acetic acid-water (35 + 5 + 60). Aspartame can be separated in the presence of caffeine and vanillin by using the mobile phase pH 3 acetate buffer-methanol (95 + 5). Retention factors and minimum detectable limits are described. The percentage error and the percent relative standard deviation for 6 replicate samples ranged from 0.3 to 2.8 and from 1.64 to 3.60, respectively. Recovery of additives added to the foods named and analyzed by the direct method and by extraction ranged from 98.0 to 100.6% and from 91.6 to 101.8%, respectively. The proposed LC techniques are simple, rapid, and advantageous because all the additives can be detected in a single step, which makes it useful for the routine analysis of various food products.

scholarly journals Simultaneous Identification and Quantification of Anthraquinones, Polydatin, and Resveratrol in Polygonum multiflorum, Various Polygonum Species, and Dietary Supplements by Liquid Chromatography and Microscopic Study of Polygonum Species

2007 ◽  
Vol 90 (6) ◽  
pp. 1532-1538 ◽  
Author(s):  
Bharathi Avula ◽  
Vaishali C Joshi ◽  
Yan-Hong Wang ◽  
Ikhlas A Khan
Keyword(s):  
Acetic Acid ◽  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Polygonum Multiflorum ◽  
Relative Standard ◽  
Simultaneous Identification ◽  
Liquid Chromatographic

Abstract A high-performance liquid chromatographic (HPLC) method with ultraviolet absorption detection was developed to determine the presence of anthraquinones, polydatin, and resveratrol in Polygonum multiflorum Thunb. as well as other medicinal Polygonum species, viz., P. cuspidatum, P. oriental, P. aviculare, and P. vulgare, as well as commercial products that claim to contain P. multiflorum. The best results were obtained with a Phenomenex Gemini C18 column using gradient mobile phase composed of water (0.1 acetic acid) and acetonitrile (0.1 acetic acid). Elution was at a flow rate of 1.0 mL/min. The detection wavelength was 280 nm for anthraquinones and 320 nm for polydatin and resveratrol. The main anthraquinones identified were emodin and physcion. The HPLC pattern of P. multiflorum was also compared with 5 other species of Polygonum. The method was validated for precision, repeatability, and accuracy. The relative standard deviation was between 0.9 and 1.6. The method was sensitive, quick, and accurate for determination of anthraquinones, polydatin, and resveratrol in 6 different species of Polygonum and can be used for quality control of P. multiflorum. The commercial samples and the 6 Polygonum species were compared microscopically, and a detailed description is provided for P. multiflorum.

Liquid Chromatographic Determination of Methyldopa and Methyldopa-Thiazide Combinations in Dosage Forms

1983 ◽  
Vol 66 (6) ◽  
pp. 1436-1442
Author(s):  
Susan Ting
Keyword(s):  
Acetic Acid ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Dosage Forms ◽  
Reverse Phase ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method, using a reverse phase C18 column, an acetic acid-methanol-water mobile phase, and detection at 280 nm, was developed for the determination of methyldopa in tablets and oral suspensions and combinations of methyldopa with hydrochlorothiazide or chlorothiazide in tablets. A mixture of these 3 drugs was resolved in <8 min. Detector responses were linear for the following amounts (mg/mL) of drug injected: methyldopa 0.031-0.393, chlorothiazide 0.019-0.114, and hydrochlorothiazide 0.004-0.083. Recoveries from commercial dosage forms ranged from 99.1 to 100.9% for methyldopa, 99.2-100.4% for chlorothiazide, and 100.0-101.2% for hydrochlorothiazide. Replicate injections of methyldopa, chlorothiazide, and hydrochlorothiazide standard preparations alone or in combination gave overall relative standard deviations of <1.6% (n = 10). The results for methyldopa tablets by the proposed method were in agreement with those obtained by the USP XX method. The LC method detected as little as 0.6 μg 3-O-methylmethyldopa/mL and 0.5 μg 4-amino-6- chloro-l,3-benzenedisulfonamide/mL, which are sometimes found as contaminants of methyldopa and thiazides, respectively, and resolved methyldopa from its methyldopa glucose adduct, a substance found in methyldopa oral suspensions.

scholarly journals Determination of Fleroxacin in Pure and Tablet Forms by Liquid Chromatography and Derivative UV-Spectrophotometry

2003 ◽  
Vol 86 (2) ◽  
pp. 229-235 ◽  
Author(s):  
Dorota Kowalczuk ◽  
Hanna Hopkała
Keyword(s):  
Mobile Phase ◽  
Internal Standard ◽  
Spectrophotometric Assay ◽  
Uv Spectrophotometry ◽  
Aminobenzoic Acid ◽  
Tetrabutylammonium Hydroxide ◽  
Relative Standard ◽  
Liquid Chromatographic ◽  
Derivative Uv Spectrophotometry

Abstract Derivative UV-spectrophotometric and liquid chromatographic (LC) methods for fleroxacin determination were validated. In the spectrophotometric assay, first-, second-, third-, and fourth-order measurements were applied with the use of peak–zero and peak–peak techniques. The linear correlation between amplitude of the peak and concentration of the examined drug ranged from 2.0 to 12.0 μg/mL. An isocratic LC analysis was performed on a Purospher ODS column with an acidic mobile phase containing tetrabutylammonium hydroxide. Measurements were made at a wavelength of 285 nm with 4-aminobenzoic acid (PABA) as internal standard. The calibration curve was linear (r = 0.9999) in the studied range of concentration (1.0–10.0 μg/mL). The accuracy (mean recovery, about 100%), precision (relative standard deviation <1%), selectivity, and sensitivity of the elaborated methods were satisfactory.

Isolation, Purification, and Liquid Chromatographic Determination of Stilbene Phytoalexins in Peanuts

1995 ◽  
Vol 78 (5) ◽  
pp. 1177-1182 ◽  
Author(s):  
Victor S Sobolev ◽  
Richard J Cole ◽  
Joe W Dorner ◽  
Boris Yagen
Keyword(s):  
Acetic Acid ◽  
Silica Gel ◽  
Mobile Phase ◽  
High Speed ◽  
Chromatographic Determination ◽  
Normal Phase ◽  
Phase Partition ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for determination of stilbene phytoalexins (SPs) in peanuts has been developed. SPs were extracted with acetonitrile–water (90 + 10, v/v) by high-speed blending. An aliquot of extract was applied to a minicolumn packed with AI2O3–ODS (C18) mixture and eluted with acetonitrile-water (90 + 10, v/v). Eluate was evaporated under nitrogen, and residue was dissolved in LC mobile phase. SPs in an aliquot of purified extract were quantitated by normal-phase partition LC on silica gel with n-heptane–2-propanol–water–acetonitrile–acetic acid (1050 + 270 + 17 + 5 + 1, v/v) as mobile phase. Recoveries of SPs [frans-4-(3-methyl-but-1-enyl)-3,5,4′-trihy-droxystilbene (trans-arachidin-3; t-Ar-3), trans-3-isopentadienyl-4,3′,5′-trihydroxystilbene (t-IPD), and trans-3,5,4′-trihydroxystilbene (trans-resveratrol; t-Res)] from peanuts spiked at 300 ppb were 96.05 ± 2.8%. Limits of quantitation for t-Ar-3 and t-IPD were about 100 ppb. t-Ar-3, t-IPD, and t-Res were found in all parts of the peanut plant as major SPs produced in response to fungal invasion.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

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.

Ultra-Performance Liquid Chromatographic and Densitometric Methods for Sensitive Determination of Xipamide and Triamterene in Pure and Pharmaceutical Dosage Forms

2021 ◽  
Author(s):  
N V Fares ◽  
Haitham A El Fiky ◽  
Amr M Badawey ◽  
Maha F Abd El Ghany
Keyword(s):  
Acetic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detection ◽  
Pharmaceutical Dosage Forms ◽  
Selective Determination ◽  
Liquid Chromatographic

Abstract Background Validated UPLC method and TLC densitometric method were prescribed for determination of antihypertensive components. Objectives: To establish and validate rapid and accurate Ultra performance liquid chromatographic (UPLC) and TLC densitometric methods for determination of Xipamide and Triamterene in pure and dosage forms. Methods The first method; UPLC method, depended on using Agilent Zorbax Eclipse Plus C8 (50 mm × 2.1 mm, 1.8 μm), as the column, mobile phase composed of (acetonitrile-water) (70 + 30, v/v) adjusted by acetic acid to obtain (pH 3), 0.2 mL/min flow rate and UV detection at 231.4 nm. The second method was a thin layer chromatography (TLC) densitometric method, separation was achieved by using toluene-methanol-ethyl chloride-acetic acid (7 + 2 + 1 + 0.2, v/v/v) as the mobile phase, pre coated silica gel plates as the stationary phase and UV detection at 300.0 nm. Results The obtained results were validated and statistically compared with official and reported methods. The obtained results showed high accuracy and reproducible results with excellent mean recoveries for both drugs. Conclusions The UPLC method showed shorter retention time for both Xipamide (0.88 min) and Triamterene (0.63 min), lower detection limit less than 0.055 µg/mL for both drugs with high selectivity, decreased injection volume (1 µL) and lower flow rate other than any HPLC method. Both proposed methods were sensitive, selective, and effectively applied to pure and dosage forms (Epitens®). Highlights Unprecedented sensitive, rapid, and reproducible UPLC and TLC methods were developed for selective determination of mixture of Xipamide and Triamterene with LOD less than 0.076 µg/mL for both drugs.

Simultaneous Determination of Xylazine and Its Major Metabolite, 2,6-Dimethylaniline, in Bovine and Swine Kidney by Liquid Chromatography

1993 ◽  
Vol 76 (4) ◽  
pp. 720-724 ◽  
Author(s):  
David C Holland ◽  
Robert K Munns ◽  
José E Roybal ◽  
Jeffrey A Hurlbut ◽  
Austin R Long
Keyword(s):  
Acetic Acid ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Sodium Acetate ◽  
Major Metabolite ◽  
Bovine Kidney ◽  
Liquid Chromatographic ◽  
Swine Kidney

Abstract A liquid chromatographic (LC) method is described for the simultaneous determination of xylazine (XY) and its major metabolite, 2,6-dimethylaniline (2,6- DMA), in bovine and swine kidney in the 25– 100 ppb range. XY and 2,6-DMA are extracted from kidney with chloroform, followed by cleanup on an acidic Celite 545 column. A μBondapak phenyl column is used for LC separation with UV determination at 225 nm. The mobile phase is a mixture of acetonitrile, water, sodium acetate, and acetic acid. Mean recoveries from bovine kidney were 78.3% for XY, with a standard deviation (SD) of 7.45 and a coefficient of variation (CV) of 9.51 %, and 87.2% for 2,6-DMA, with an SD of 8.38 and a CV of 9.61 %. Mean recoveries from swine kidney were 80.8% for XY, with an SD of 5.92 and a CV of 7.33%, and 86.7% for 2,6-DMA, with an SD of 6.16 and a CV of 7.10%.

Liquid Chromatographic Determination of Dicofol in Kelthane Formulations: Collaborative Study

1986 ◽  
Vol 69 (4) ◽  
pp. 714-720
Author(s):  
Alan M Rothman ◽  
◽  
A Ausari ◽  
O O Bennett ◽  
E J Blusiewicz ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Standard Deviation ◽  
High Resolution ◽  
Mobile Phase ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
In Series ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method was used to determine p,p'- and o,p'-isomers of dicofol AI (active ingredient) in Kelthane® EC and MF formulations. Samples are dissolved in methanol and AI components and impurities are separated on a high resolution C8 column in series with a short C18 guard column, with a methanol-water-acetic acid mobile phase. Cleaned samples are directly injected into the LC system and are monitored at 254 nm. Twelve collaborators submitted results on 5 samples. Using 95% confidence criteria, the average total standard deviation of the total AI across all samples was 2.82%. The method has been adopted official first action.

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