Development of a new high performance low pressure chromatographic system using a multisyringe burette coupled to a chromatographic monolithic column

This paper presents a new application for monolithic columns with low-pressure chromatographic separation using an flow injection analysis configuration with chemiluminescent detection for the determination of a mixture of phenolic compounds: phloroglucinol, 2,4-dihydroxybenzoic acid, salicylic acid, methyl paraben and n-propyl gallate. The procedure consists of the separation of these compounds on a reverse-phase ultra-short monolithic column with pH 3.0 acetate buffer and 5% acetonitrile as carrier phase. The detection is based on a chemiluminescence measurement coming from Ce(IV)-Rhodamine 6G chemistry with the incorporation of two different chemiluminescent chemical conditions in the chromatographic setup in order to enhance the sensitivity for the different phenolic compounds. All separation and detection variables were optimized to propose a determination method. The analysis is performed in 280?s, with the sampling frequency being some 13 h(-1) . The calibration function is a double reciprocal function obtaining good results within two orders of magnitude. The limits of detection were 8.8 × 10 (-8) m (phloroglucinol), 2.7 × 10 (-8) m (2,4-dihydroxybenzoic acid); 2.3 × 10 (-8) m (salicylic acid); 5.2 × 10 (-8) m (methyl paraben) and 4.1 × 10 (-6) m (n-propyl gallate), and the relative standard deviations at a medium level of the linear range were 4.4% (phloroglucinol), 2.8% (2,4-dihydroxybenzoic acid), 5.2% (salicylic acid), 3.6% (methyl paraben) and 6.8% (n-propyl gallate). The method was applied and validated satisfactorily for the determination of these compounds in healthcare products, comparing the results against an HPLC reference method.

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Analysis of phenolic compounds in health care products by low‐pressure liquid‐chromatography with monolithic column and chemiluminescent detection

Ballesta-Claver

Valencia

Capitán-Vallvey

2011

Luminescence

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Development and validation of a method to determine amoxicillin in physiological fluids using micellar liquid chromatography

Rambla-Alegre

Carda‐Broch

Romero³

2008

J of Separation Science

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Abbreviations MLC micellar liquid chromatographyFDA food and drug analysis 2 Abstract A simple and robust method was developed for the routine identification and quantification of amoxicillin by micellar liquid chromatography. Amoxicillin, a β-lactamase inhibitor, is one of the most commonly prescribed drugs in the treatment of urine and skin structure infections. In this work, amoxicillin was determined in urine samples without any pretreatment step in a phenyl column using a micellar mobile phase of 0.10 M sodium dodecyl sulfate and 4% butanol at pH 3. A UV detection set at 210 nm was used. Amoxicillin is eluted at 5.1 min with no interference by the protein band or endogenous compounds. Linearities (r > 0.9998), intra-and inter-day precisions were determined (RSD (%) 0.4-2.7% and 0.3-5%, respectively in micellar media, and 0.14-2.6% and 0.13-6%, respectively in urine), and robustness was studied in the validation of the method. LOD and LOQ were 0.06 and 0.4 µg/mL in micellar media and 0.11 and 0.4 µg/mL in urine, respectively. Recoveries in the urine matrix were in the range of 95-110%. The validated method proved to be reliable and sensitive for the determination of amoxicillin in urine samples.

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Modulation of mobile phase composition in flow-injection/sequential-injection chromatography exploiting multisyringe flow analysis

et al. 2008

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In this paper, a time-based multicommutated flow system is proposed for appropriate selection and modulation of mobile phase composition in flow-injection (FI)/sequential-injection (SI) chromatography. The novel flow assembly involves the on-line coupling of a short monolithic reversed-phase chromatographic column with a multisyringe flow injection set-up furnished with a set of solenoid valves. The proposed hyphenated technique was applied to the simultaneous spectrophotometric determination of thiamine (B(1)), pyridoxine (B(6)) and cyanocobalamin (B(12)) which were taken as model analytes. The separation method capitalizes on a dual isocratic elution protocol involving the use of a single forward stroke of the multisyringe pump for initial delivery of 50 mmol L(-1) ammonium acetate (pH 7.0) for 2.4 min followed by 50 mmol L(-1) ammonium acetate-methanol (80:20, v/v) for 6.4 min at 0.5 mL min(-1) and room temperature. Detection was performed at the maximum wavelength for each target vitamin-280 nm for B(1), 325 nm for B(6), and 360 nm for B(12). A first-order, two-level full-factorial design was utilized to ascertain the significant variables influencing the chromatographic separation and the magnitude of the interaction effects. The experimental design method revealed that resolution of the target vitamins is highly dependent on the pH, percentage of organic modifier, and their second-order interaction. The multisyringe flow-injection-based monolithic column separation method, which should be viewed as an expeditious and cost-effective alternative to the high-performance liquid chromatography counterpart, was applied to the separation and determination of B(1), B(6), and B(12) in different pharmaceutical dosage forms in less than 9 min. Statistical comparison of the results from the proposed procedure with those from the HPLC method endorsed by the US Pharmacopeia revealed there were no significant differences at the 95% confidence level.

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Development of a new high performance low pressure chromatographic system using a multisyringe burette coupled to a chromatographic monolithic column

Cited by 33 publications

References 9 publications

Analysis of phenolic compounds in health care products by low‐pressure liquid‐chromatography with monolithic column and chemiluminescent detection

Analysis of phenolic compounds in health care products by low‐pressure liquid‐chromatography with monolithic column and chemiluminescent detection

Development and validation of a method to determine amoxicillin in physiological fluids using micellar liquid chromatography

Modulation of mobile phase composition in flow-injection/sequential-injection chromatography exploiting multisyringe flow analysis

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