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Switchable‐hydrophilicity solvent liquid‐liquid microextraction versus dispersive liquid‐liquid microextraction prior to HPLC‐UV for the determination and isolation of piperine from Piper nigrum L
Authors:Mais Al‐Nidawi,Usama Alshana,Jude Caleb,Malek Hassan,Zia ur Rahman,Duygu Yi  it Hano  lu,&#x  hsan   al&#x    
Affiliation:Mais Al‐Nidawi,Usama Alshana,Jude Caleb,Malek Hassan,Zia ur Rahman,Duygu Yiğit Hanoğlu,İhsan Çalış
Abstract:
Switchable‐hydrophilicity solvent liquid‐liquid microextraction and dispersive liquid‐liquid microextraction were compared for the extraction of piperine from Piper nigrum L. prior to its analysis by using high‐performance liquid chromatography with UV detection. Under optimum conditions, limits of detection and quantitation were found as 0.2–0.6 and 0.7–2.0 μg/mg with the two methods, respectively. Calibration graphs showed good linearity with coefficients of determination (R2) higher than 0.9962 and percentage relative standard deviations lower than 6.8%. Both methods were efficiently used for the extraction of piperine from black and white pepper samples from different origins and percentage relative recoveries ranged between 90.0 and 106.0%. The results showed that switchable‐hydrophilicity solvent liquid‐liquid microextraction is a better alternative to dispersive liquid‐liquid microextraction for the routine analysis of piperine in food samples. A novel scaled‐up dispersive liquid‐liquid microextraction method was also proposed for the isolation of piperine providing a yield of 102.9 ± 4.9% and purity higher than 98.0% as revealed by NMR spectroscopy.
Keywords:black pepper  dispersive liquid‐liquid microextraction  piperine  switchable‐hydrophilicity solvent  white pepper
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