Search

A novel microporous membrane/solvent microextraction (MPMSME) approach was developed in which a piece of microporous filter membrane was used as not only extraction solvent holder but also solid phase extraction unit. Subsequently, high-performance liquid chromatography with an UV detector was conducted. The wide exchange surface and very little organic solvent consumption made this sample pretreatment technology very interesting. The cinnamic acid derivatives were used as model analytes to evaluate the procedure. Parameters that affect the MPMSME such as type of extraction solvent, membrane area (or volumes of extraction solvent), aqueous phase pH, ionic strength, extraction stirring rate, extraction time, and sample volume were investigated and optimized. The enrichment factor (EF) of analyte was defined in MPMSME. Under the optimized conditions, the EFs of cinnamic acid derivatives were 43–144. Good linearities were obtained from 4 to 4,000 ng mL−1 for all the analytes with regression coefficients of between 0.9956 and 0.9977; the limits of quantification were below 0.4 ng mL−1, and satisfactory recoveries (93–106 %) and precisions (0.37–13 %) were also achieved. The experimental results showed that the method was simple, rapid, practical, and effective for preconcentration and determination of the cinnamic acid derivatives in rhizoma typhonii.

An advantageous method based on hollow fiber liposome microscreening (HFLMS) combined with high-performance liquid chromatography (HPLC) has been developed and used in preliminary screening and analysis of biomembrane permeable compounds from herbal medicines (HMs). In the method, a liposome hollow fiber was prepared as a screening tool; permeable compounds that could specifically bind to liposomes were screened from herbal extract to liposome in the pores and lumen of hollow fiber, then permeable compounds were dissociated from liposomes and analyzed by HPLC. The chromatographic separation was applied with a Zorbax Eclipse XDB-C18 column by a gradient elution using acetonitrile, methanol, and phosphoric acid aqueous solution as the mobile phases. In the study, influencing factors of the screened target compounds were investigated and optimized. Under optimum conditions, the surface properties of liposome hollow fibers were characterized, the nonspecific binding between the active center of hollow fiber and the bioactive components were investigated, the repeatability of this method was tested. And eight permeable compounds of flavonoids and anthraquinones from HMs were preliminarily screened and analyzed by HFLMS-HPLC. The results demonstrated that new method is a simple, fast, effective, and reliable method for preliminary screening and analyzing biomembrane permeable ingredients in HMs, and it can be used in screening other permeable compounds in HMs.

In this paper, two methods, organic solvent dispersive liquid–liquid microextraction (OS-DLLME) and ionic liquid dispersive liquid–liquid microextraction (IL-DLLME), coupled with high-performance liquid chromatography have been critically compared and introduced for the analysis of the eight coumarin compounds (psoralen, isopsoralen, bergapten, isobergapten, oxypeucedanin, imperatorin, osthole, and isoimperatorin) in Radix Angelicae Dahuricae samples. Experimental conditions have been investigated for both OS-DLLME and IL-DLLME. Under optimal conditions, the detection limits of the eight coumarin compounds obtained by OS-DLLME and IL-DLLME ranged between 0.002–0.026 ng mL−1 and 0.013–0.66 ng mL−1, respectively. The relative standard deviations (RSDs, n = 9) were lower than 8.7 and 8.4% with enrichment factors in the range of 145–380 and 130–230 folds for OS-DLLME and IL-DLLME, respectively. The results showed that there were no significant deviations between the two DLLME methods for the determination of the eight coumarin compounds. Both methods were simple, fast, efficient, and inexpensive. However, compared with IL-DLLME, the OS-DLLME technique exhibited a higher extraction capacity for the eight target analytes.

Hollow fiber liquid–liquid phase microextraction followed by high-performance liquid chromatography was employed to research the binding of four furocoumarin compounds (psoralen, oxypeucedanin, imperatorin and isoimperatorin) to bovine serum albumin. The results reveal that the percent of drug–protein binding did not rely on the furocoumarins and protein concentrations, and four furocoumarins scarcely competed for protein binding sites. The protein-binding percents of psoralen, oxypeucedanin, imperatorin and isoimperatorin were 55.1 ± 4.5, 14.4 ± 2.4, 44.1 ± 6.7, and 41.3 ± 3.8%, respectively, the numbers of binding sites were 1.2, 1.6, 0.6 and 0.3, and the binding constants were 1,801, 212, 937 and 4,025 L mol−1, respectively. The proposed new approach is simple, rapid, and effective for the study of the interaction between protein and furocoumarin compounds which is either individual or coexistent with the similar ones.