Separation of inorganic anions by capillary electrophoresis (CE) is usually conducted in co-electroosmotic mode due to the large electrophoretic mobilities of inorganic anions. Semipermanent surfactant coatings have been shown to be effective for CE of inorganic anions due to their strong capability of electroosmotic flow (EOF) manipulation. However, semipermanent coatings often suffer from their unsatisfactory stability. In addition, organic solvent additives are usually required to adjust the selectivity, which also aggravate the degradation of coating. In this work, a novel semipermanent coating consisting of cationic Gemini surfactant 18-10-18 and nonionic surfactant Tween 20 was developed to separate inorganic anions in CE. This coating is easy to prepare and more stable than pure Gemini coating. The introduction of nonionic surfactant in the coating not only suppresses the reversed EOF but can also adjust the selectivity of separation. Good separations of six model anions were achieved, the separation efficiency was as high as 65040–169700 plates/m and the RSDs of the migration times were less than 0.5 and 2.5% for run-to-run and day-to-day assays, respectively. Calibration curves were linear in the range of 0.05−5.0 mM; the detection limits ranged from 20 to 50 μM. More importantly, no organic solvents are required in the background buffer to achieve the satisfactory separations. This guarantees the coating stability and makes the method greener than most of other methods for CE of inorganic anions.

Ionic liquid surfactants are a class of ionic liquids (ILs), which can form micelles in the aqueous solution. In this paper, we demonstrate a novel extracting system based on the use of IL surfactants in ultrasonic-assisted extraction followed by HPLC analysis. No organic solvents were used in the extraction, making this method environmentally friendly and more attractive than the conventional organic solvent-based extraction methods. As an example, this method was applied to determine tanshinones in Chinese herbal medicine Salvia miltiorrhiza bunge. The effect of the carbon chain length of the IL cation, as well as other influencing factors on ultrasonic-assisted extraction, was investigated in detail. Under the optimized conditions, satisfactory extraction efficiency was achieved with the recoveries ranging from 87.5 to 107.6%, and the RSDs were lower than 6%. This work shows a promising prospect of the IL surfactants in the extraction of active ingredients from herbs.

This paper proposes a new method for CE separation of inorganic anions based on the use of gemini surfactants as capillary coatings in mixed aqueous-organic solvents. The semipermanent gemini surfactant coatings were facilely prepared by rinsing the capillary with 18-s-18 solutions; they can keep be stable during the electrophoretic runs without surfactants in buffer. The coatings showed a good tolerance of methanol (MeOH) or ACN, e.g. at pH 8.0 and with 40% v/v MeOH or ACN, the EOF magnitude after 60 min of continuous electrokinetic rinsing only decreased by 2.9 or 6.0%, respectively. The coatings were successfully applied to the separation of inorganic anions. Adding organic solvents in buffer can effectively improve the resolution and efficiencies; however, it remarkably prolonged the analysis time due to the suppression of EOF. Interestingly, varying the spacer length of the gemini surfactants can also modulate (improve) the resolution but without any sacrifice of analysis time. This benefit was resulted from the unique chemical structures of gemini surfactants because it introduced a new variable, i.e. the spacer length, to the separation mechanism.

Layer-by-layer (LBL) assembly is a versatile nanofabrication technique, and investigation of its kinetics is essential for understanding the assembly mechanism and optimizing the assembly procedure. In this work, the LBL assembly of polyelectrolyte and nanoparticles were monitored in situ by capillary electrophoresis (CE) for the first time. The assembly of poly(diallyldimethylammonium chloride) (PDDA), and gold nanoparticles (AuNPs) on capillary walls causes surface-charge neutralization and resaturation, and thus yields synchronous changes in the electroosmotic flow (EOF). The EOF data show that formation of multilayers follows first-order adsorption kinetics. On the basis of the fit results, influencing factors, including number of layers, concentration of materials, flow rate, and size of AuNPs, were investigated. The stability and robustness of the assembled coatings were also characterized by CE. It was found that degradation of PDDA layers follows first-order chemical kinetics, while desorption of AuNPs takes place in a disorderly manner. The substrate strongly affects assembly of the underlying layer, while this effect is rapidly screened with increasing number of layers. Furthermore, we demonstrate that the EOF measuring step does not disturb LBL assembly, and the proposed method is reliable and rugged. This work not only studies in detail the LBL adsorption/desorption process of polyelectrolyte and nanoparticles, but also offers an alternative tool for monitoring multilayer buildup. It may also reveal the potential of CE in fields other than analytical separation.

Recently, amino acid ionic liquids (AAILs) have attracted much research interest. In this paper, we present the first application of AAILs in chiral separation based on the chiral ligand exchange principle. By using 1-alkyl-3-methylimidazolium L-proline (L-Pro) as a chiral ligand coordinated with copper(II), four pairs of underivatized amino acid enantiomers—dl-phenylalanine (dl-Phe), dl-histidine (dl-His), dl-tryptophane (dl-Trp), and dl-tyrosine (dl-Tyr)—were successfully separated in two major chiral separation techniques, HPLC and capillary electrophoresis (CE), with higher enantioselectivity than conventionally used amino acid ligands (resolution (R_s)=3.26–10.81 for HPLC; R_s=1.34–4.27 for CE). Interestingly, increasing the alkyl chain length of the AAIL cation remarkably enhanced the enantioselectivity. It was inferred that the alkylmethylimidazolium cations and L-Pro form ion pairs on the surface of the stationary phase or on the inner surface of the capillary. The ternary copper complexes with L-Pro are consequently attached to the support surface, thus inducing an ion-exchange type of retention for the dl-enantiomers. Therefore, the AAIL cation plays an essential role in the separation. This work demonstrates that AAILs are good alternatives to conventional amino acid ligands for ligand-exchange-based chiral separation. It also reveals the tremendous application potential of this new type of task-specific ILs.

N-(2-Phenyl-indolyl)-acetic acid (PIAA), a new fluorescent derivatizing reagent, was used for the determination of diethylene glycol (DEG) by high-performance liquid chromatography with fluorescence detection. DEG was derivatized to ester by using PIAA in the presence of 1-ethyl-3-(3-dimethylaminopropyl)carbodimide hydrochloride (as dehydrating agent) and 4-(dimethylamino)pyridine (as base catalyst) in acetonitrile at 60°C for 75 min. The influence of solvent, temperature, catalyst base, concentration of labeling reagent, and couple reagent on the derivatization was investigated. The fluorescence detection was performed with excitation at 340 nm and emission at 377 nm. Baseline separation was obtained on an Ultimate XB-C18 analytical column with water/acetonitrile gradient elution, good linearity was obtained within 0.5–50 μg/mL with a correlation coefficient of 0.9997. The limit of detection was 0.01 μg/mL (signal-to-noise ratio = 3). The method has been successfully applied to determine DEG in toothpaste samples with satisfactory recoveries ranging from 89.0 to 94.9%. The proposed method was shown to be a promising technique for the determination of DEG with high sensitivity.