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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

Chromatograms for the analysis of tramadol in urine samples. (a) HPLC chromatogram of the urine sample (volunteer with abuse of tramadol) spiked with tramadol at concentration level 60 μg/ Lafter employing BS-DLLME, (b) HPLC chromatogram of blank human urine sample (healthy volunteer) after performing BS-DLLME. Extraction conditions: tramadol concentration, 100 μg/L; binary extraction solvents and their volume, 100 μL mixture of ethyl acetate and chloroform (3:7 v/v); disperser solvent and its volume, 0.6 mL acetone; 7.5% NaCl.
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Figure 8: Chromatograms for the analysis of tramadol in urine samples. (a) HPLC chromatogram of the urine sample (volunteer with abuse of tramadol) spiked with tramadol at concentration level 60 μg/ Lafter employing BS-DLLME, (b) HPLC chromatogram of blank human urine sample (healthy volunteer) after performing BS-DLLME. Extraction conditions: tramadol concentration, 100 μg/L; binary extraction solvents and their volume, 100 μL mixture of ethyl acetate and chloroform (3:7 v/v); disperser solvent and its volume, 0.6 mL acetone; 7.5% NaCl.

Mentions: Representative chromatograms with good resolution obtained for tramadol, from blank human urine sample (healthy volunteer) and urine sample (volunteer with abuse of tramadol) spiked with tramadol under the optimum BS-DLLME condition are shown in Figure 8.


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)

Chromatograms for the analysis of tramadol in urine samples. (a) HPLC chromatogram of the urine sample (volunteer with abuse of tramadol) spiked with tramadol at concentration level 60 μg/ Lafter employing BS-DLLME, (b) HPLC chromatogram of blank human urine sample (healthy volunteer) after performing BS-DLLME. Extraction conditions: tramadol concentration, 100 μg/L; binary extraction solvents and their volume, 100 μL mixture of ethyl acetate and chloroform (3:7 v/v); disperser solvent and its volume, 0.6 mL acetone; 7.5% NaCl.
© Copyright Policy - open-access
Related In: Results  -  Collection

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

Figure 8: Chromatograms for the analysis of tramadol in urine samples. (a) HPLC chromatogram of the urine sample (volunteer with abuse of tramadol) spiked with tramadol at concentration level 60 μg/ Lafter employing BS-DLLME, (b) HPLC chromatogram of blank human urine sample (healthy volunteer) after performing BS-DLLME. Extraction conditions: tramadol concentration, 100 μg/L; binary extraction solvents and their volume, 100 μL mixture of ethyl acetate and chloroform (3:7 v/v); disperser solvent and its volume, 0.6 mL acetone; 7.5% NaCl.
Mentions: Representative chromatograms with good resolution obtained for tramadol, from blank human urine sample (healthy volunteer) and urine sample (volunteer with abuse of tramadol) spiked with tramadol under the optimum BS-DLLME condition are shown in Figure 8.

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