This paper presents at first time that the ultra-performance™ liquid chromatographic atmospheric pressure chemical ionization mass spectrometer (UPLC-APCI-MS) was used as an efficient method for the identification and quantification of diversiform phytosterols in food materials. The sample preparation consisted of extraction by supercritical carbon dioxide fluid extraction (SCE) and saponification by refluxing with ethanolic KOH, and then the non-saponificable fraction was extracted with petroleum ether. This fraction was subjected to solid phase extraction (SPE) on silica gel cartridge and then the sterols were eluted with hexane-ethyl acetate. Sterols were separated on an Acquity UPLC™ BEH C18 column (100 mm × 1.0 mm, 1.7 μm particle size) with a gradient of methanol/water (1% acetonitrile) at a flow of 0.1 mL min−1. The determination was performed in selective ion monitoring mode. The quality parameter of the developed method was established using 6-ketocholestanol as internal standard. Limits of quantification (LOQ) were 0.1754, 0.0341, 0.0500, 0.0205, 0.0225, 0.3674, 0.0241, 0.0272, 0.0076 μg L−1 and 0.1525 μg mL−1 for 6-ketocholestanol, desmosterol, ergosterol, cholesterol, lanosterol, cholestanol, campesterol, stigmasterol, β-sitosterol, and stigmastanol, respectively. The intra- and inter-day determination precision for the 10 phytosterols were less than 5 and 6% in relative standard deviations, and their recoveries were located in the range of 94-107%. The developed approach has been applied successfully for efficient determination of diversiform phytosterols in food materials, including corn, sesame, oat and peanut. 相似文献
Iron sulfides with different atomic ratios were synthesized by a hydrothermal method and used to modify a glassy carbon electrode. The various sulfides were compared to each other for their amperometric response to H2O2. It is found that FeS is the most adequate material. Operated in 0.1 M NaOH solution at 0.4 V (vs. Ag/AgCl), the sensor based on FeS displays a linear response that extends from 0.50 μM to 20.5 mM of H2O2, with a sensitivity of 36.4 μA mM?1 cm?2 and a detection limit of 0.15 μM (at an S/N ratio of 3). The sensor is selective, stable and reproducible.
Graphical abstract Schematic of the synthesis of pomegranate flower-like FeS by a hydrothermal route using ferric chloride and thiourea (SC(NH2)2) as the precursors, and ethanolamine (EA) as the structure-guiding auxiliary agent. A glassy carbon electrode (GCE) modified with this material allows for amperometric sensing of hydrogen peroxide in 0.1 M NaOH solution with a 0.15 μM detection limit.
Research on Chemical Intermediates - To explore the potential impacts of nanoscale zero-valent iron (nZVI) particles on nitrite accumulation performance of nitritation granular sludge (NGS), two... 相似文献
This paper addresses the rate-distortion (R-D) optimal packetization (RDOP) of embedded bitstreams into independent source packets, in order to limit error propagation in transmission of images over packet noisy channels. The input embedded stream is assumed to be an interleaving of K independently decodable basic streams. To form independent source packets, the set of basic streams is partitioned into N groups. The streams within each group are then interleaved to generate a source packet. Error/erasure protection may be further applied along/across source packets, to produce the channel packets to be transmitted. The RDOP problem previously formulated by Wu et at. has the goal of finding the partitioning that minimizes the distortion when all source packets are decoded. We extend the problem formulation such that to also include the minimization of the expected distortion for general transmission scenarios that may apply uneven erasure/ error protection. Further, we show that the dynamic programming (DP) algorithm of Wu et al. can be extended to solve the general RDOP problem. The main contribution of this paper is a fast divide-and-conquer algorithm (D&C) to find the globally optimal solution, under the assumption that all basic streams have convex R-D curves. Instrumental in obtaining the fast solution is our result which proves that the problem can be formulated as a series of matrix search problems in totally monotone matrices. The proposed D&C reduces the running time from O(K(2)LN) where L is the size of each packet achieved by the DP solution to O(NKL log K). Experiments on SPIHT coded images demonstrate that the speedup is significant in practice. 相似文献