TY - JOUR
T1 - Method validation and determinations of levofloxacin, metronidazole and sulfamethoxazole in an aqueous pharmaceutical, urine and blood plasma samples using quantitative nuclear magnetic resonance spectrometry
AU - Salem, Alaa A.
AU - Mossa, Hussein A.
PY - 2012/1/15
Y1 - 2012/1/15
N2 - Selective, rapid and accurate quantitative proton nuclear magnetic resonance (qHNMR) method for the determination of levofloxacin, metronidazole benzoate and sulfamethoxazole in aqueous solutions was developed and validated. The method was successfully applied to the determinations of the drugs and their admixtures in pharmaceutical, urine and plasma samples. Maleic acid and sodium malate were used as internal standards. Effect of temperature on spectral measurements was evaluated. Linear dynamic ranges of 0.50-68.00, 0.13-11.30 and 0.24-21.00 mg per 0.60 mL solution were obtained for levofloxacin, metronidazole benzoate and sulfamethoxazole, respectively. Average recovery % in the range of 96.00-104.20 ± (0.17-2.91) was obtained for drugs in pure, pharmaceutical, plasma and urine samples. Inter and intra-day analyses gave average recoveries % in the ranges 96.10-98.40 ± (1.68-2.81) and 96.00-104.20 ± (0.17-2.91), respectively. Instrumental detection limits ≤0.03 mg per 0.6 mL were obtained for the three drugs. Developed method has demonstrated high performance characteristics for analyzing investigated drugs and their admixtures. Student t-test at 95% confidence level revealed insignificant bias between the real and measured contents of investigated drugs in pure, pharmaceutical, urine and plasma samples and its admixtures. Application of the statistical F-test revealed insignificant differences in precisions between the developed method and arbitrary selected reference methods.
AB - Selective, rapid and accurate quantitative proton nuclear magnetic resonance (qHNMR) method for the determination of levofloxacin, metronidazole benzoate and sulfamethoxazole in aqueous solutions was developed and validated. The method was successfully applied to the determinations of the drugs and their admixtures in pharmaceutical, urine and plasma samples. Maleic acid and sodium malate were used as internal standards. Effect of temperature on spectral measurements was evaluated. Linear dynamic ranges of 0.50-68.00, 0.13-11.30 and 0.24-21.00 mg per 0.60 mL solution were obtained for levofloxacin, metronidazole benzoate and sulfamethoxazole, respectively. Average recovery % in the range of 96.00-104.20 ± (0.17-2.91) was obtained for drugs in pure, pharmaceutical, plasma and urine samples. Inter and intra-day analyses gave average recoveries % in the ranges 96.10-98.40 ± (1.68-2.81) and 96.00-104.20 ± (0.17-2.91), respectively. Instrumental detection limits ≤0.03 mg per 0.6 mL were obtained for the three drugs. Developed method has demonstrated high performance characteristics for analyzing investigated drugs and their admixtures. Student t-test at 95% confidence level revealed insignificant bias between the real and measured contents of investigated drugs in pure, pharmaceutical, urine and plasma samples and its admixtures. Application of the statistical F-test revealed insignificant differences in precisions between the developed method and arbitrary selected reference methods.
KW - Levofloxacin
KW - Method validation
KW - Metronidazole benzoate
KW - Plasma
KW - Quantitative HNMR
KW - Sulfamethoxazole
KW - Urine
UR - http://www.scopus.com/inward/record.url?scp=84855974752&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=84855974752&partnerID=8YFLogxK
U2 - 10.1016/j.talanta.2011.10.016
DO - 10.1016/j.talanta.2011.10.016
M3 - Article
C2 - 22265475
AN - SCOPUS:84855974752
SN - 0039-9140
VL - 88
SP - 104
EP - 114
JO - Talanta
JF - Talanta
ER -