Method development and validation for trifluoroacetic acid determination by capillary electrophoresis in combination with capacitively coupled contactless conductivity detection (CE-C4D).
Summary of "Method development and validation for trifluoroacetic acid determination by capillary electrophoresis in combination with capacitively coupled contactless conductivity detection (CE-C4D)."
A method was developed to determine traces of trifluoroacetic acid as impurity in synthetic or semi-synthetic drugs as antibiotics, macropeptides, etc. Capillary electrophoresis in combination with capacitively coupled contactless conductivity detection (CE-C(4)D) was used due to lack of UV absorbance property of trifluoroacetic acid (TFA). The optimized method took less than 1 min with good linearity (R(2)=0.9995) for trifluoroacetic acid concentration from 2 to 100 ppm. It also has a good repeatability expressed by the relative standard deviation (% RSD) which is 1.2 and 2.1% for intraday and interday precision, respectively, at 50 ppm TFA, and good sensitivity with 0.34 ppm, 1.2 ppm LOD and LOQ, respectively. In addition, the content of TFA in synthetic drug, was determined using the validated method which gave good linearity (R(2)=0.9996) for trifluoroacetic acid spiked into drug in a concentration range of 2-80 ppm, with good intraday repeatability of 2.0%. The analysis is performed in a background electrolyte composed of 20mM morpholinoethane-sulfonic acid (Mes) and 20mM L-histidine (L-His) pH 6.1. Cetyltrimethylammonium bromide (CTAB) was added as flow modifier in a concentration (0.2mM) lower than the critical micellar concentration. Ammonium formate 6 ppm was used as internal standard. The applied voltage was 30 kV in reverse polarity. A fused silica capillary with 75 μm internal diameter and total length 47 cm (31 cm to C(4)D detector and 37 cm to DAD detector) was used.
Affiliation
Laboratory for Pharmaceutical Analysis, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, O & N 2, PB 923, Herestraat 49, B-3000 Leuven, Belgium.
Journal Details
This article was published in the following journal.
Name: Talanta
ISSN: 1873-3573
Pages: 400-3
Links
- PubMed Source: http://www.ncbi.nlm.nih.gov/pubmed/21111152
- DOI: http://dx.doi.org/10.1016/j.talanta.2010.09.051
Medical and Biotech [MESH] Definitions
Capillary Electrochromatography
A separation technique which combines LIQUID CHROMATOGRAPHY and CAPILLARY ELECTROPHORESIS.
Trifluoroacetic Acid
A very strong halogenated derivative of acetic acid. It is used in acid catalyzed reactions, especially those where an ester is cleaved in peptide synthesis.
Electrophoresis, Capillary
A highly-sensitive (in the picomolar range, which is 10,000-fold more sensitive than conventional electrophoresis) and efficient technique that allows separation of PROTEINS; NUCLEIC ACIDS; and CARBOHYDRATES. (Segen, Dictionary of Modern Medicine, 1992)
Sex Determination (analysis)
Validation of the SEX of an individual by inspection of the GONADS and/or by genetic tests.
Sex Determination Analysis
Validation of the SEX of an individual by inspection of the GONADS and/or by genetic tests.
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