Liquid Chromatographic Separations Using Rubber as the Stationary Phase

1963 ◽  
Vol 36 (1) ◽  
pp. 310-312
Author(s):  
P. I. Brewer

Abstract In a previous communication it was reported that certain polymers could be separated from mineral oil by a liquid chromatographic method. n-Heptane was used as the mobile phase and small pieces of thin vulcanized natural latex as the stationary phase. It has now been found that compounds of lower molecular weight can also be separated by this method. The use of rubber for the separation of compounds of low molecular weight was first described by Boldingh; he found it advantageous first to swell the rubber with a different solvent from that used as the mobile phase. The use of a crosslinked dextran (“Sephadex”) for separating compounds in aqueous solution has been described by Gelotte. Vaughan has mentioned the possibility of using crosslinked polystyrene beads for this purpose.

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.


Author(s):  
Udayasree Konikuru ◽  
Rajavel P. ◽  
Vijitha S.

Objective: A simple, selective, precise and accurate method was developed for the estimation of Clozapine by RP-HPLC technique.Methods: Chromatographic conditions used are stationary phase, Phenomenex BDS (150 mm x 4.6 mm, 5µ), Mobile phase was methanol and water in (80:20) ratio and flow rate was maintained at 1.0 ml/min, column temperature was set at 25 °C, detection wavelength was 240 nm, and diluent was mobile phase. These conditions were finalized for the optimized method.Results: Linearity study was carried out between 10-60 µg/ml, the R2 value was found to be as 0.995. Precision was found to be as follows for system precision 1.052, method precision 1.662, and intraday precision 1.02 and for interday precision 0.93. The % Recovery was found to be 98.60%. LOD and LOQ were found to be 2.7 µg/ml and 8.4 µg/ml respectively. By using the above method assay of the marketed formulation was carried out and the % purity was found to be 99.28 %. Stability studies of Clozapine were done, in all conditions degradation was found to be within the acceptable range.Conclusion: The current validated method was finally applied in bioequivalence studies of four different brands of Clozapine by using dissolution apparatus and percentage drug release was found to be 99.48%, it was within the acceptable limit (NLT 85 %) as per USP.


1986 ◽  
Vol 69 (6) ◽  
pp. 1026-1030
Author(s):  
Bruce C Flann ◽  
Bruce A Lodge

Abstract The validation of a liquid chromatographic procedure suitable for the determination of calcitriol and alfacalcidol in their respective formulations labeled to contain at least 0.25 μ.g drug per unit is described. The capsule content is diluted and chromatographed in 15-20 min on silica columns (5 μm) with a mobile phase of hexane-tetrahydrofuranmethylene dichloride-isopropanol (72 + 12 + 12 + 4, v/v) with detection at 254 nm. The calibration curve is linear. Recoveries of “spikes” averaged 101% with a standard deviation of 2%. Precision was better than 1.5%.


2009 ◽  
Vol 92 (3) ◽  
pp. 846-854 ◽  
Author(s):  
Phyllis Wilson

Abstract Progesterone and estrogens are hormones produced in the human body that are essential for regulating many vital functions. The three major estrogens produced by women are estriol, estradiol, and estrone. Progesterone is a naturally occurring hormone in both men and women. Pharmaceuticals containing estrogens alone or estrogens in combination with progesterone are commonly used in therapy. Patients requiring unique combinations of the drugs rely on pharmacies to compound the ingredients. In order to assess the potency of drugs containing combinations of estrogens and progesterone, a method was developed to determine all four ingredients simultaneously. The liquid chromatographic method utilized a Bondapak C18 column with an isocratic mobile phase of acetonitrilewater (50 + 50, v/v) at a flow rate of 1.0 mL/min and temperature of 30C. Under these conditions, the order of elution was estriol, estradiol, and estrone, followed by progesterone. UV detection was at 205 nm to monitor elution of the estrogens, then switched to 270 nm to monitor progesterone. The method was applied to the analysis of pharmacy-compounded drugs containing combinations of the hormones. Validation studies demonstrated that the method is accurate and precise.


1993 ◽  
Vol 76 (1) ◽  
pp. 92-94 ◽  
Author(s):  
Paolo Cabras ◽  
Marinella Melis ◽  
Lorenzo Spanedda

Abstract A liquid chromatographic method is described for the determination of cymiazole residues in honey. This acaricide is determined on a reversed-phase (C18) column, with a CH3CN-O.OOIN HCI-NaCI mixture (950 mL + 50 mL + 0.3 g/L) as the mobile phase, and UV detection at 265 nm. Cymiazole is extracted with n-hexane from aqueous alkalinized (pH 9) honey solutions. No further cleanup of the honey extract was required before chromatographic analysis. Recoveries on control samples fortified with 0.01,0.10, and 1.00 ppm cymiazole ranged from 92 to 102%. The limit of determination was 0.01 ppm.


2005 ◽  
Vol 88 (4) ◽  
pp. 1086-1092 ◽  
Author(s):  
Fanny L B Guerra ◽  
Clesio S Paim ◽  
Martin Steppe ◽  
Elfrides E S Schapoval

Abstract A microbiological assay and a liquid chromatographic method were validated for quantitation of moxifloxacin in tablets. The microbiological method consisted of a cylinder-plate agar diffusion assay using Micrococcus luteus ATCC 9341 as the test microorganism and phosphate buffer (0.1M, pH 8.0) as the diluent solution. The response graphs for standard and sample solutions were linear (r = 0.9479), and no parallelism deviations were detected in the tested levels of concentration (4.0, 8.0, and 16.0 μg/mL). The interday precision was 2.73%. Recovery values were between 96.25 and 100.5%. The chromatographic analyses were performed using a Shim-pack CLC-ODS column (250 × 4.6 mm, 5 μm) with a mobile phase consisting of (A) a mixture of phosphoric acid (0.17%, v/v) with tetramethylammonium hydroxide (0.05M) and acetonitrile (95 + 5, v/v) and (B) methanol (55 + 45, v/v) adjusted to pH 3.0. The flow rate was 1.0 mL/min, and detection was made at 294 nm. The method was linear in a range from 12.0 to 42 μg/mL (r = 0.9999), and the interday precision was 1.39%. Recovery ranged between 101.9 and 103. 81%. Both validated methods were used to quantify the moxifloxacin content in tablets exposed to ultraviolet radiation, and similar results were obtained.


2000 ◽  
Vol 83 (4) ◽  
pp. 789-792 ◽  
Author(s):  
Ehab A Abourashed ◽  
Ikhlas A Khan

Abstract The migraine prophylactic herb feverfew (Tanacetum parthenium L.) is marketed in the United States in a variety of forms and compositions. Although its therapeutic efficacy is still uncertain, the sesquiterpene lactone parthenolide is the constituent recommended to be measured for quality control of feverfew preparations. A validated liquid chromatographic method was developed and used to estimate parthenolide in a number of U.S. feverfew market products formulated as capsules, tablets, or crude powder. The method uses a Lichrosphere 5 C18 column, a mobile phase consisting of 50mM NaH2PO4 in H2O (solvent A), and CH3CN–MeOH (90 + 10, v/v; solvent B). Elution was run at a flow rate of 1.0 mL/min with a linear gradient of 50–15% A in B over 20 min and UV detection at 210 nm. The correlation coefficient for the calibration curve was 0.9999 over the range of 0.00–0.400 mg/mL. Overall recovery of parthenolide was 103.1%.


1987 ◽  
Vol 42 (9) ◽  
pp. 1187-1194 ◽  
Author(s):  
Michael Nieder ◽  
Halvor Jaeger

A high performance liquid chromatographic method was developed to study the pharmacokinetics of nicergoline and its two main m etabolites in humans. The analytes are extracted from blood, plasma and urine into a mixture of chloroform and ether, which is optimised in terms of recovery and absence of interferences. The analytes are separated on a small bore column filled with octadecylsilica. the mobile phase was a ternary mixture of water, acetonitrile and tetrahydrofurane with diisopropylamine for pH adjustment. To maintain the chromatographic stability. the mobile phase is circulated and a saturator column inserted between pump and sampler. Nicergoline is very unstable in blood, it could not be determined in human body fluids after a single dose of 10 mg nicergoline. Metabolite 1 reaches plasma concentrations of about 2 ng/ml after 40 min. metabolite 2 gains to about 8 ng/ml after 4 h. 67% of the dosed nicergoline are excreted in urine as free metabolite 2. free metabolite 1 occurred only in trace concentrations. 18.5% of the dosed drug were excreted as conjugated metabolite 2. 1.1% as conjugated metabolite 1.


Author(s):  
Chaitanya A. Gulhane ◽  
Wrushali A. Panchale ◽  
Jagdish V. Manwar ◽  
Ravindra L. Bakal

A new simple, reproducible and efficient liquid chromatographic method (RP-HPLC) was developed for simultaneous estimation of thiocolchicoside and etoricoxib for tablet formulation. Formulation containing thiocolchicoside and etoricoxib is used as analgesic. Separation was achieved by Nucleosil (4.6mm I.D × 250 mm) C18 column with mobile phase consist of Acetonitrile: water (0.05% Orthophosphoric acid V/V) in the ratio 25:75 at flow rate 0.7ml . The detection was carried out at 220nm. The retention time of thiocolchicoside and etoricoxib was found to be 3.75 min and 6.13 min respectively. Linearity of THC and ETR was found to be in the range of 2-10µg/mL and 30-150µg/mL. Percent recovery obtained for THC and ETR were 99.98% and 99.69% respectively. The method was validated as per ICH guidelines.


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