Study Of Ionic Liquid-based Liquid-phase Microextraction Of Pharmaceutical Analysis

The separation and analysis of trace components in complex matrices is a difficult problem in pharmaceutical analysis,which plays an important role in drug development,dosage form research and metabolic analysis.Separation and enrichment are the key steps to improve the sensitivity of complex matrix analysis.Traditional extraction technology has some disadvantages,such as high dosage of organic solvents,toxicity,time-consuming and low recovery.It has become the most important thigh for drug analysis to seek a sample pretreatment technology with high enrichment capacity,safety,environmental protection and simplicity.In recent years,with the rapid development of ionic liquid,which has high selectivity,less dosage,designable,various,and environment friendly advantages and gradually be seriously,a series of liquid phase microextraction techniques based on ionic liquid have become the new trend in pharmaceutical analysis.In this paper,based on the nature of the different types of ionic liquids,choose suitable ionic liquids as the extraction solvent,and liquid phase microextraction and high performance liquid chromatography（HPLC）was used to determine the antibiotics and traditional Chinese medicine in blood.Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid microextraction system was developed and applied to the extraction of sulfonamides in blood.High-performance liquid chromatography was applied to the determination of the analytes.The blood sample was centrifuged to obtain the serum.After the proteins in the serum were removed in the presence of acetonitrile,ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate,dipotassium hydrogen phosphate,ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution.After the resulting mixture was ultrasonically shaken and centrifuged,the precipitate was separated.The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase.The parameters affecting the extraction efficiency,such as volume of ionic liquid,amount of dipotassium hydrogen phosphate,volume of dispersion solvent,extraction time and temperature were investigated.The limits of detection of sulfamethizole,sulfachlorpyridazine,sulfamethoxazole and Sulfisoxazole were 4.78,3.99,5.21 and3.77μg L^-1,respectively.When this method was applied to the analysis of real blood samples,the recoveries of analytes ranged from 91.0%to 111.6%and relative standard deviations were lower than 7.0%.Ionic liquid/anionic surfactant aqueous two-phase system was developed and applied for the extraction of sulfonamides in blood.,and high-performance liquid chromatography（HPLC）was applied to the determination of the analytes.The blood sample was centrifuged and added to sodium dodecyl sulfate（SDS）,ionic liquid1-Hexyl-3-MethylImidazolium Chloride（[C₆MIM]Cl）,K₂HPO₄.The mixture was ultrasonically shaken and centrifuged,and the aqueous two phase system was formed,the analytes were extracted into the upper phase.The parameters affecting the extraction efficiency,such as volume of ionic liquid,amount of sodium dodecyl sulfate,ionic strength,pH value of system,extraction time and temperature were investigated.The limits of detection of Sulfamethyldiazine,Sulfamethizole,sulfachlorpyridazine,sulfamethoxazole and Sulfisoxazole were 3.29,4.13,3.74,2.45and 3.60μg L^-11 respectively.When the present method was applied to the analysis of real blood samples,the recoveries of analytes ranged from 86.4 to 116.3%and relative standard deviations were lower than 6.9%.Green,rapid,and simple method,ionic-liquid-magnetized stirring bar liquid-phase microextraction was developed for the determination of naphthoquinones,including shikonin andβ,β′-dimethylacrylshikonin in Zicao.The method is uesd to combine magnetic stirring,extraction,and pre-enrichment in a single device simultaneously,so the extract is conveniently collected.The analytes were extracted from the sample to ionic liquid-magnetized stirring bar,then the analyte-adsorbed magnetized stirring bar can be readily isolated from the sample solution by a magnet.The key experimental parameters were investigated and optimized,including the type and volume of ionic liquid,extraction time,salt concentration,stirring speed,and pH.The recoveries were in the range of 89.47–102.38%,and good reproducibilities were obtained with relative standard deviation below 5.36%.Compared with the conventional extraction methods,the proposed method is quicker and more effective.