Limits...
Binary Solvents Dispersive Liquid-Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography.

Kiarostami V, Rouini MR, Mohammadian R, Lavasani H, Ghazaghi M - Daru (2014)

Bottom Line: The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively.The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6).Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Chemistry, North Tehran Branch, Islamic Azad University, P,O, Box 1913674711, Tehran, Iran. v_kiarostami@iau-tnb.ac.ir.

ABSTRACT

Background: Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase.

Results: Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 - 99.6%.

Conclusions: Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

No MeSH data available.


Related in: MedlinePlus

Effect of high density extraction solvent type on the extraction efficiency. Extraction condition: tramadol concentration, 100 μg/ L; volume of extraction solvent, 50 μL; disperser solvent and its volume, 0.6 mL acetonitrile; no salt addition.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
getmorefigures.php?uid=PMC3924918&req=5

Figure 1: Effect of high density extraction solvent type on the extraction efficiency. Extraction condition: tramadol concentration, 100 μg/ L; volume of extraction solvent, 50 μL; disperser solvent and its volume, 0.6 mL acetonitrile; no salt addition.

Mentions: Selection of high density extraction solvent is very important in BS-DLLME procedure. For this purpose chloroform (CHCl3, density 1.49 g/L), carbon tetrachloride (CCl4, density 1.59 g/ml) and dichloromethane (CH2Cl2, density 1.32 gmL−1) selected in this study. A series of urine samples were surveyed by using 0.6 mL of acetone (as disperser solvent) contains 70 μL of different high density extraction solvents. In the presence of dichloromethane as extraction solvent, no droplet was formed and therefore ignored as extraction solvent. As shown in Figure 1, chloroform has better extraction recovery with significant effect (unpaired t-test assuming unequal variances, p < 0.05) than the other tested solvents. Therefore, CHCl3 was selected as the extraction solvent in subsequent experiments.


Binary Solvents Dispersive Liquid-Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography.

Kiarostami V, Rouini MR, Mohammadian R, Lavasani H, Ghazaghi M - Daru (2014)

Effect of high density extraction solvent type on the extraction efficiency. Extraction condition: tramadol concentration, 100 μg/ L; volume of extraction solvent, 50 μL; disperser solvent and its volume, 0.6 mL acetonitrile; no salt addition.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3924918&req=5

Figure 1: Effect of high density extraction solvent type on the extraction efficiency. Extraction condition: tramadol concentration, 100 μg/ L; volume of extraction solvent, 50 μL; disperser solvent and its volume, 0.6 mL acetonitrile; no salt addition.
Mentions: Selection of high density extraction solvent is very important in BS-DLLME procedure. For this purpose chloroform (CHCl3, density 1.49 g/L), carbon tetrachloride (CCl4, density 1.59 g/ml) and dichloromethane (CH2Cl2, density 1.32 gmL−1) selected in this study. A series of urine samples were surveyed by using 0.6 mL of acetone (as disperser solvent) contains 70 μL of different high density extraction solvents. In the presence of dichloromethane as extraction solvent, no droplet was formed and therefore ignored as extraction solvent. As shown in Figure 1, chloroform has better extraction recovery with significant effect (unpaired t-test assuming unequal variances, p < 0.05) than the other tested solvents. Therefore, CHCl3 was selected as the extraction solvent in subsequent experiments.

Bottom Line: The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively.The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6).Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Chemistry, North Tehran Branch, Islamic Azad University, P,O, Box 1913674711, Tehran, Iran. v_kiarostami@iau-tnb.ac.ir.

ABSTRACT

Background: Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase.

Results: Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 - 99.6%.

Conclusions: Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

No MeSH data available.


Related in: MedlinePlus