Caffeine analysis in urine by gas chromatography mass spectrometry: A non-derivatization detection and confirmatory method

Eylem Funda Göktaş; Erol Kabil

Makale detayları

Caffeine analysis in urine by gas chromatography mass spectrometry: A non-derivatization detection and confirmatory method

Yazarlar:

Eylem Funda Göktaş | Erol Kabil

Yayıncı:

Istanbul University

Ana Başlıklar:

Pharmaceutical Analytical Chemistry

Dergi:

İstanbul Journal of Pharmacy Vol.54 Issue 2, pp.233-239

Belge Tipi:

Makale

Yayın Tarihi:

8/2024

Belge Dili:

İngilizce

Document ID (Org No.):

2001329754

pISSN:

2587-2087

Anahtar kelimeler:

Özet:

 Background and Aims: Caffeine is a xanthine alkaloid found naturally in plants. Caffeine has cardiotonic and stimulant effects in humans and animals. For this reason, caffeine is on the monitoring list for human sports and is listed as a feed contaminant in horse racing. The aim of this study was to develop a rapid, practical, and specific method for the determination of caffeine in horse urine. Methods: In the new method, the pH of the sample was adjusted by the addition of phosphate buffer, and after solid phase extraction, it was dissolved in methanol before being analysed by gas chromatography mass spectrometry without derivatization. The method was validated according to the European Commissions 2002657EC criteria. Results: The effects of different cartridge brands, pH, and elution solution were determined. Intraday and interday CV values are 2.8 and 5.2 for the International Residue Limit IRL, respectively. Five levels blank, 0.5xIRL, IRL, 1.5xIRL, and 2xIRL were used in constructing the curve, and the R2 value was greater than 0.99. The analysis run was 11.8 min. The decision limit CCα was determined to be 56.7 ngmL due to IRL. The detection limit of the method was calculated to be 3.3 ngmL. The method was determined to be robust according to changes in extraction pH, phosphate buffer concentration, centrifugation time, hexane volume in the wash step, different grades of methanol, inlet temperature, and operator. Conclusion: The applicability of the method was demonstrated by analysing positive and negative horse urine samples. Validation parameters showed the method to be selective, specific, and easy to apply.

 Background and Aims: Caffeine is a xanthine alkaloid found naturally in plants. Caffeine has cardiotonic and stimulant effects in humans and animals. For this reason, caffeine is on the monitoring list for human sports and is listed as a feed contaminant in horse racing. The aim of this study was to develop a rapid, practical, and specific method for the determination of caffeine in horse urine. Methods: In the new method, the pH of the sample was adjusted by the addition of phosphate buffer, and after solid phase extraction, it was dissolved in methanol before being analysed by gas chromatography mass spectrometry without derivatization. The method was validated according to the European Commissions 2002657EC criteria. Results: The effects of different cartridge brands, pH, and elution solution were determined. Intraday and interday CV values are 2.8 and 5.2 for the International Residue Limit IRL, respectively. Five levels blank, 0.5xIRL, IRL, 1.5xIRL, and 2xIRL were used in constructing the curve, and the R2 value was greater than 0.99. The analysis run was 11.8 min. The decision limit CCα was determined to be 56.7 ngmL due to IRL. The detection limit of the method was calculated to be 3.3 ngmL. The method was determined to be robust according to changes in extraction pH, phosphate buffer concentration, centrifugation time, hexane volume in the wash step, different grades of methanol, inlet temperature, and operator. Conclusion: The applicability of the method was demonstrated by analysing positive and negative horse urine samples. Validation parameters showed the method to be selective, specific, and easy to apply.

 Background and Aims: Caffeine is a xanthine alkaloid found naturally in plants. Caffeine has cardiotonic and stimulant effects in humans and animals. For this reason, caffeine is on the monitoring list for human sports and is listed as a feed contaminant in horse racing. The aim of this study was to develop a rapid, practical, and specific method for the determination of caffeine in horse urine. Methods: In the new method, the pH of the sample was adjusted by the addition of phosphate buffer, and after solid phase extraction, it was dissolved in methanol before being analysed by gas chromatography mass spectrometry without derivatization. The method was validated according to the European Commissions 2002657EC criteria. Results: The effects of different cartridge brands, pH, and elution solution were determined. Intraday and interday CV values are 2.8 and 5.2 for the International Residue Limit IRL, respectively. Five levels blank, 0.5xIRL, IRL, 1.5xIRL, and 2xIRL were used in constructing the curve, and the R2 value was greater than 0.99. The analysis run was 11.8 min. The decision limit CCα was determined to be 56.7 ngmL due to IRL. The detection limit of the method was calculated to be 3.3 ngmL. The method was determined to be robust according to changes in extraction pH, phosphate buffer concentration, centrifugation time, hexane volume in the wash step, different grades of methanol, inlet temperature, and operator. Conclusion: The applicability of the method was demonstrated by analysing positive and negative horse urine samples. Validation parameters showed the method to be selective, specific, and easy to apply.

 Background and Aims: Caffeine is a xanthine alkaloid found naturally in plants. Caffeine has cardiotonic and stimulant effects in humans and animals. For this reason, caffeine is on the monitoring list for human sports and is listed as a feed contaminant in horse racing. The aim of this study was to develop a rapid, practical, and specific method for the determination of caffeine in horse urine. Methods: In the new method, the pH of the sample was adjusted by the addition of phosphate buffer, and after solid phase extraction, it was dissolved in methanol before being analysed by gas chromatography mass spectrometry without derivatization. The method was validated according to the European Commissions 2002657EC criteria. Results: The effects of different cartridge brands, pH, and elution solution were determined. Intraday and interday CV values are 2.8 and 5.2 for the International Residue Limit IRL, respectively. Five levels blank, 0.5xIRL, IRL, 1.5xIRL, and 2xIRL were used in constructing the curve, and the R2 value was greater than 0.99. The analysis run was 11.8 min. The decision limit CCα was determined to be 56.7 ngmL due to IRL. The detection limit of the method was calculated to be 3.3 ngmL. The method was determined to be robust according to changes in extraction pH, phosphate buffer concentration, centrifugation time, hexane volume in the wash step, different grades of methanol, inlet temperature, and operator. Conclusion: The applicability of the method was demonstrated by analysing positive and negative horse urine samples. Validation parameters showed the method to be selective, specific, and easy to apply.

Makale detayları

Caffeine analysis in urine by gas chromatography mass spectrometry: A non-derivatization detection and confirmatory method

Yazarlar:

Eylem Funda Göktaş | Erol Kabil

Yayıncı:

Istanbul University

Ana Başlıklar:

Pharmaceutical Analytical Chemistry

Dergi:

İstanbul Journal of Pharmacy Vol.54 Issue 2, pp.233-239

Belge Tipi:

Makale

Yayın Tarihi:

8/2024

Belge Dili:

İngilizce

Document ID (Org No.):

2001329754

pISSN:

2587-2087

Caffeine

Gas chromatography-mass spectrometry

Urine

Sayı

Makale detayları

Caffeine analysis in urine by gas chromatography mass spectrometry: A non-derivatization detection and confirmatory method

Yazarlar: Eylem Funda Göktaş | Erol Kabil

Yayıncı: Istanbul University

Ana Başlıklar: Pharmaceutical Analytical Chemistry

Dergi: İstanbul Journal of Pharmacy Vol.54 Issue 2, pp.233-239

Belge Tipi: Makale

Yayın Tarihi: 8/2024

Belge Dili: İngilizce

Document ID (Org No.): 2001329754

pISSN: 2587-2087

Caffeine

Gas chromatography-mass spectrometry

Urine

Sayı

Yazarlar:

Eylem Funda Göktaş | Erol Kabil

Yayıncı:

Istanbul University

Ana Başlıklar:

Pharmaceutical Analytical Chemistry

Dergi:

İstanbul Journal of Pharmacy Vol.54 Issue 2, pp.233-239

Belge Tipi:

Makale

Yayın Tarihi:

8/2024

Belge Dili:

İngilizce

Document ID (Org No.):

2001329754

pISSN:

2587-2087