SPE and large-volume sample stacking in MEKC for determination of doxycycline in biological fluids: Comparison of direct injection to SPE-MEKC
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2008
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A novel and simple method has been developed for the determination of doxycycline (DOX) in biological fluids. The method is based on SPE, large-volume sample stacking (LVSS) and MEKC with UV-DAD detection. Six SPE cartridges have been used in investigation for sample clean up and pre-concentration (Supelco (R) LC-8, LC-18, LC-SCX, and LC-WCX, as well as Strata (TM)-X and X-C). DOX was determined on a 56 cm. (effective length 50 cm) x 50 mu m id fused-silica capillary. The BGE was 20 mM borate buffer, pH 9.3, containing 80 mM SDS and 7.5% v/v of methanol (30 s x 50 mbar), and the temperature and voltage were 25 degrees C and 30 kV, respectively. The analytical wavelength was set at 210 nm. Under optimized conditions it is possible to determine DOX in human serum, urine, semen, tears and saliva with recovery of 97.5% (RSD 2.5%). The method was shown to be sensitive (LOD is 1 mu g/L) and precise (intra-day RSD 0.2 and 2.4%; inter-days 0.4 and 3.5% for migration time and peak area, respect...ively). Results for developed SPE-LVSS-MEKC were compared with LVSS-MEKC method with direct sample injection. The new LVSS-MEKC method is presented as a useful technique for rapid determination without extraction procedure of DOX in human urine and serum, using 80mM of SDS, 10% v/v of methanol and 40 mM borate buffer (pH 9.3; 30 s x 50 mbar; 25 degrees C; 30 kV; 350 nm), but not for the other biological fluids, according to lower sensitivity of the method and because of the sample composition.
Ključne reči:
Biological fluids / Direct injection / Doxycycline / LVSS / SPE-MEKCIzvor:
Electrophoresis, 2008, 29, 21, 4431-4438Izdavač:
- Wiley-VCH Verlag GMBH, Weinheim
Finansiranje / projekti:
- Supstance za farmaceutsku upotrebu: modeliranje, sinteza, fizičko-hemijske i biološke osobine, stepen čistoće i ispitivanje doziranih oblika (RS-MESTD-MPN2006-2010-142072)
DOI: 10.1002/elps.200800339
ISSN: 0173-0835
PubMed: 18956436
WoS: 000261484100019
Scopus: 2-s2.0-59249109357
Institucija/grupa
PharmacyTY - JOUR AU - Injac, Rade AU - Karljiković-Rajić, Katarina AU - Štrukelj, Borut PY - 2008 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1061 AB - A novel and simple method has been developed for the determination of doxycycline (DOX) in biological fluids. The method is based on SPE, large-volume sample stacking (LVSS) and MEKC with UV-DAD detection. Six SPE cartridges have been used in investigation for sample clean up and pre-concentration (Supelco (R) LC-8, LC-18, LC-SCX, and LC-WCX, as well as Strata (TM)-X and X-C). DOX was determined on a 56 cm. (effective length 50 cm) x 50 mu m id fused-silica capillary. The BGE was 20 mM borate buffer, pH 9.3, containing 80 mM SDS and 7.5% v/v of methanol (30 s x 50 mbar), and the temperature and voltage were 25 degrees C and 30 kV, respectively. The analytical wavelength was set at 210 nm. Under optimized conditions it is possible to determine DOX in human serum, urine, semen, tears and saliva with recovery of 97.5% (RSD 2.5%). The method was shown to be sensitive (LOD is 1 mu g/L) and precise (intra-day RSD 0.2 and 2.4%; inter-days 0.4 and 3.5% for migration time and peak area, respectively). Results for developed SPE-LVSS-MEKC were compared with LVSS-MEKC method with direct sample injection. The new LVSS-MEKC method is presented as a useful technique for rapid determination without extraction procedure of DOX in human urine and serum, using 80mM of SDS, 10% v/v of methanol and 40 mM borate buffer (pH 9.3; 30 s x 50 mbar; 25 degrees C; 30 kV; 350 nm), but not for the other biological fluids, according to lower sensitivity of the method and because of the sample composition. PB - Wiley-VCH Verlag GMBH, Weinheim T2 - Electrophoresis T1 - SPE and large-volume sample stacking in MEKC for determination of doxycycline in biological fluids: Comparison of direct injection to SPE-MEKC VL - 29 IS - 21 SP - 4431 EP - 4438 DO - 10.1002/elps.200800339 ER -
@article{ author = "Injac, Rade and Karljiković-Rajić, Katarina and Štrukelj, Borut", year = "2008", abstract = "A novel and simple method has been developed for the determination of doxycycline (DOX) in biological fluids. The method is based on SPE, large-volume sample stacking (LVSS) and MEKC with UV-DAD detection. Six SPE cartridges have been used in investigation for sample clean up and pre-concentration (Supelco (R) LC-8, LC-18, LC-SCX, and LC-WCX, as well as Strata (TM)-X and X-C). DOX was determined on a 56 cm. (effective length 50 cm) x 50 mu m id fused-silica capillary. The BGE was 20 mM borate buffer, pH 9.3, containing 80 mM SDS and 7.5% v/v of methanol (30 s x 50 mbar), and the temperature and voltage were 25 degrees C and 30 kV, respectively. The analytical wavelength was set at 210 nm. Under optimized conditions it is possible to determine DOX in human serum, urine, semen, tears and saliva with recovery of 97.5% (RSD 2.5%). The method was shown to be sensitive (LOD is 1 mu g/L) and precise (intra-day RSD 0.2 and 2.4%; inter-days 0.4 and 3.5% for migration time and peak area, respectively). Results for developed SPE-LVSS-MEKC were compared with LVSS-MEKC method with direct sample injection. The new LVSS-MEKC method is presented as a useful technique for rapid determination without extraction procedure of DOX in human urine and serum, using 80mM of SDS, 10% v/v of methanol and 40 mM borate buffer (pH 9.3; 30 s x 50 mbar; 25 degrees C; 30 kV; 350 nm), but not for the other biological fluids, according to lower sensitivity of the method and because of the sample composition.", publisher = "Wiley-VCH Verlag GMBH, Weinheim", journal = "Electrophoresis", title = "SPE and large-volume sample stacking in MEKC for determination of doxycycline in biological fluids: Comparison of direct injection to SPE-MEKC", volume = "29", number = "21", pages = "4431-4438", doi = "10.1002/elps.200800339" }
Injac, R., Karljiković-Rajić, K.,& Štrukelj, B.. (2008). SPE and large-volume sample stacking in MEKC for determination of doxycycline in biological fluids: Comparison of direct injection to SPE-MEKC. in Electrophoresis Wiley-VCH Verlag GMBH, Weinheim., 29(21), 4431-4438. https://doi.org/10.1002/elps.200800339
Injac R, Karljiković-Rajić K, Štrukelj B. SPE and large-volume sample stacking in MEKC for determination of doxycycline in biological fluids: Comparison of direct injection to SPE-MEKC. in Electrophoresis. 2008;29(21):4431-4438. doi:10.1002/elps.200800339 .
Injac, Rade, Karljiković-Rajić, Katarina, Štrukelj, Borut, "SPE and large-volume sample stacking in MEKC for determination of doxycycline in biological fluids: Comparison of direct injection to SPE-MEKC" in Electrophoresis, 29, no. 21 (2008):4431-4438, https://doi.org/10.1002/elps.200800339 . .