[Stable isotope ratio characteristics and origin tracing of Portunus trituberculatus]. / ä¸åŒäº§åœ°ä¸‰ç–£æ¢­å­èŸ¹çš„ç¨³å®šåŒä½ç´ æ¯”å€¼ç‰¹å¾åŠåŽŸäº§åœ°æº¯æº.

A method for geographical discrimination of Portunus trituberculatus was explored to provide technical support for the protection of geographical indication products and for tracing the origin of seafood. P. trituberculatus were collected from three major production areas, including the Yellow Sea, the Bohai Sea, and the East China Sea. The variations of carbon and nitrogen stable isotope values of origins and the correlation of stable isotope ratios in different tissues were analyzed. The results showed that there were significant differences in carbon and nitrogen stable isotope ratio among different origins. Significant isotope fractionation effects were observed among different tissues. The discriminant model was developed and the origin discriminant analysis was performed by the stable isotope ratios of different tissues in P. trituberculatus. The correct rate of origin diffe-rentiationf using carbon and nitrogen stable isotopes in muscle and gills (>95%) was significantly higher than that of hepatopancreas and gonad, indicating that stable isotope ratios of muscle and gills could effectively differentiate P. trituberculatus in different sea areas. This study filled the gap of stable isotope tracing technology for P. trituberculatus.

Simultaneous determination of malachite green, crystal violet, methylene blue and the metabolite residues in aquatic products by ultra-performance liquid chromatography with electrospray ionization tandem mass spectrometry.

This work describes solid-phase extraction-ultra-performance liquid chromatography with electrospray ionization tandem spectrometry for determination of malachite green and metabolite leucomalachite green, crystal violet and metabolite leucocrystal violet, methylene blue and metabolites including azure A, azure B and azure C in aquatic products. Samples were extracted with acetonitrile and ammonium acetate buffer and purified by liquid extraction with dichloromethane, and then on MCAX solid-phase extraction cartridges. Then the extract was evaporated at 45°C by nitrogen blow. The residue was dissolved and separated by an Acquity BEH C18 column. The mobile phase was acetonitrile (A) and 5 mmol/L of ammonium acetate containing 0.1% formic acid (B). Analytes were confirmed and quantified using a tandem mass spectrometry system in multiple reaction mode with triple quadrupole analyzer using positive polarity mode. The limits of detection of malachite green, leucomalachite green, crystal violet and leucocrystal violet were 0.15 µg/kg, the limits of quantification were 0.50 µg/kg, and the average recoveries were more than 75% with spiked residues from 0.5 to 10 µg/kg. The relative standard deviations were less than 13%. The limits of detection of methylene blue, azure A, azure B and azure C were 0.3 µg/kg, the limits of quantification were 1.0 µg/kg, the average recoveries were more than 70% with spiked residues from 1.0 to 10 µg/kg and the relative standard deviations were less than 15%. The method has the merits of simplicity, sensitivity and rapidity, and can be used for simultaneous determination of the analytes in aquatic products.

Determination of active ingredients in corn silk, leaf, and kernel by capillary electrophoresis with electrochemicaI detection.

Corn has been known for its accumulation of flavones and phenolic acids. However, many parts of corn, except kernel, have not drawn much attention. In this work, a method based on capillary zone electrophoresis with electrochemical detection has been used for the separation and determination of epicatechin, rutin, ascorbic acid (Vc), kaempferol, chlorogenic acid, and quercetin in corn silk, leaf, and kernel. The distribution comparison of the ingredients among silk, leaf, and kernel is discussed. Several important factors--including running buffer acidity, separation voltage, and working electrode potential--were evaluated to acquire the optimum analysis conditions. Under the optimum conditions, the analytes could be well separated within 19 min in a 40-mmol/L borate buffer (pH 9.2). The response was linear over three orders of magnitude with detection limits (S/N = 3) ranging from 4.97 x 10(-8) to 9.75 x 10(-8) g/mL. The method has been successfully applied for the analysis of corn silk, leaf, and kernel with satisfactory results.