Comparison of clonidine and cyproheptadine determination in animal-derived foods by sweeping-micellar electrokinetic chromatography and large volume sample stacking-capillary zone electrophoresis

This study establishes a method for rapid detection of clonidine and cyproheptadine in foods of animal origin. In order to obtain the best detection method, capillary zone electrophoresis (CZE), large volume sample stacking (LVSS), and sweeping-micellar electrokinetic capillary chromatography (sweeping-MEKC) were used respectively. The limits of detection (LODs) of clonidine and cyproheptadine by LVSS-CZE were 0.028 μg mL−1 and 0.034 μg mL−1, and those by sweeping-MEKC were 0.023 μg mL−1 and 0.031 μg mL−1, respectively. Compared with the CZE method, the two online pre-concentration technologies have greatly improved the detection sensitivity and achieved good enrichment results. However, compared with the sweeping-MEKC system, the LVSS system consumed a longer time and was greatly affected by the actual sample matrix. The sweeping-MEKC method was proved to be suitable for real sample analysis. Under the best sweeping-MEKC conditions, clonidine and cyproheptadine could be well separated within 8 min and good linear relationships in the range of 0.1–1.0 μg mL−1 (r 2 > 0.99) were obtained. This method was successfully applied to the determination of clonidine and cyproheptadine in animal-derived foods with the recoveries of 82.3%–90.1% and the relative standard deviations (RSDs) less than 3.11%. The sweeping-MEKC method is simple to operate and has great potential in the rapid detection of clonidine and cyproheptadine in animal-derived foods.

Sample stacking – Capillary electrophoretic determination of nitrate and nitrite contents as nitric oxide metabolites in honey varieties originated from Anatolia

Nitrate and nitrite ions taken from food are the sources of bioavailable nitric oxide (NO) in the nitrogen cycle. Some beneficial effects of honey on health are attributed to the ability of honey to increase NO production. The variation of nitrate and nitrite levels of honey samples collected from different Anatolia regions were clarified using capillary electrophoresis technique. The sensitivities of both anions were improved with the application of the sample stacking method. Separation buffer consisted of 30 mmol L−1 formic acid and 30 mmol L−1 sodium sulfate at a pH of 4.0. The CE technique revealed that 18 honey samples contained nitrate anion ranged between 2.53 and 31.8 mg kg−1. Nitrite amounts were found in lower amounts in the honey samples as between non-detected and 0.533 mg kg−1. The observed differences in nitrate levels between honey varieties may be a way to determine honey's origin.

Simultaneous Separation and Analysis of Five Compounds in Cibotium barometz by Micellar Electrokinetic Chromatography with Large-Volume Sample Stacking

A large volume sample stacking (LVSS) method in micellar electrokinetic chromatography (MEKC) with diode array detector was developed for the simultaneous separation and analysis of five compounds: protocatechuic acid, protocatechuic aldehyde, caffeic acid, syringetin and vanillin in Cibotium barometz. The electrophoretic separation was performed in a 10 mM sodium dodecyl sulfate (SDS) and 50 mM sodium borax-sodium dihydrogen phosphate system (pH = 8.5) with 10% methanol at a separation voltage of 30 kV after optimizing the typical parameters. The detection limits were from 32 pg to 65 pg, which were around 12–27 times lower than MEKC, and 500 times less than reported methods. Finally, the established method was validated to be applicable for the determination of protocatechuic acid and caffeic acid in Cibotium barometz. This proposed method is expected to facilitate the quality control of Cibotium barometz.

Offline Selective Extraction Combined with Online Enrichment for Sensitive Analysis of Chondroitin Sulfate by Capillary Electrophoresis

A capillary electrophoresis (CE) method combined with online and offline enrichment for improving the detection sensitivity of chondroitin sulfate (CS) is established. The online enrichment method is based on the field-amplified sample stacking and large volume electrokinetic injection, and offline enrichment is based on the association between cetyltrimethylammonium chloride and CS. Experimental parameters affecting CE method such as the type and pH of background electrolyte, the injection mode and time and the steps of offline enrichment were optimized. Under optimum conditions, the calibration plot between CS concentration and peak area was linear in the range of 1 ~ 100 μg/mL. The enrichment factor was 130 times and the limit of detection was 50 ng/mL. The average recovery was 103.5% and the relative standard deviation of peak area was <2.0%. The method was successfully applied to the quantitative analysis of CS in drugs.