An analytical method for prohexadione in Chinese cabbage and apple

A residual determination method as a regulatory residue method was developed using HPLC‐UVD for prohexadione residues in Chinese cabbage (Brassica pekinensis) and apple (Malus domestica). The developed method consisted of solid–liquid extraction with acidic acetonitrile and ion‐suppression liquid–liquid partitioning, followed by anion exchange cartridge cleanup. The limits of detection and quantitation for the method were 0.005 and 0.02 mg/kg, respectively. The method gave good linearity in the range of 0.02–2.5 mg/kg. Accuracy and precision ranged from 84.1 to 94.1% and from 2.4 to 6.9%, respectively. Additionally, the confirmative conditions of LC‐MS/MS for prohexadione were set in negative electrospray ionization mode with transitions of m/z 211.4 → 167.5 and m/z 211.4 → 123.5 in the selected reaction monitoring mode. The applicability of the method was demonstrated by analyzing real samples collected from local markets in Seoul, Republic of Korea. This developed method fully deserves consideration in accordance with its sensitivity, accuracy and precision required for residue analysis of prohexadione in Chinese cabbages and apples. Copyright © 2010 John Wiley & Sons, Ltd.     

Solid-phase synthesis of enantio-controlled lactic acid oligomers

A synthetic method for lactic acid oligomers via solid-phase synthesis under mild reaction conditions with up to 99% yield is presented. The fine control of the chirality on each lactic acid unit of the oligomers was easily achieved by the substitution of (R)-THP-protected lactic acid (R)-2 by (S)-2 without alternating the procedure. The overall synthesis of the trimer and tetramer was completed in one and two days, respectively. Intramolecular cyclizations of enantio-controlled lactic acids were also attempted through the Yamaguchi macrolactonization or the Mitsunobu reaction. However, we were unable to isolate single cyclic oligomers but always obtained a mixture of cyclic oligomers.     

Synthesis of some 2-substituted-thioxanthones

This paper presents the synthesis of 2-amino-, 2-acetamido- and 2-benzamidothioxanthones and their 10,10-dioxides.     

SERS decoding of micro gold shells moving in microfluidic systems

In this study, in situ surface‐enhanced Raman scattering (SERS) decoding was demonstrated in microfluidic chips using novel thin micro gold shells modified with Raman tags. The micro gold shells were fabricated using electroless gold plating on PMMA beads with diameter of 15 μm. These shells were sophisticatedly optimized to produce the maximum SERS intensity, which minimized the exposure time for quick and safe decoding. The shell surfaces produced well‐defined SERS spectra even at an extremely short exposure time, 1 ms, for a single micro gold shell combined with Raman tags such as 2‐naphthalenethiol and benzenethiol. The consecutive SERS spectra from a variety of combinations of Raman tags were successfully acquired from the micro gold shells moving in 25 μm deep and 75 μm wide channels on a glass microfluidic chip. The proposed functionalized micro gold shells exhibited the potential of an on‐chip microfluidic SERS decoding strategy for micro suspension array.     

Multiresidue analysis of pesticides with hydrolyzable functionality in cooked vegetables by liquid chromatography tandem mass spectrometry

It would be preferable for pesticide residues substituted by hydrolyzable functionality to be analyzed after cooking because their structures are apt to degrade during boiling and/or heating. A liquid chromatography–tandem mass spectrometry (LC‐MS/MS) method for the quantitative determination of 44 pesticide residues with hydrolyzable functional group in five typical vegetable widely consumed in Republic of Korea is described. The sample clean‐up was carried out according to the method of Food Code No. 83 established by the Korea Food and Drug Administration (KFDA). Zorbox XDB‐C₁₈ column was selected for the analysis because of the best peak separation. The LC mobile phase consisted of water and 5 mm methanolic ammonium formate, which resulted in a peak shape with good symmetry at each run. Tandem mass spectroscopic (MS/MS) experiments were performed in ESI positive mode and the multiple reaction monitoring modes. A conventional matrix effect was modified to more comprehensive form 100γ_ij (%). A high matrix effect (相似文献   

Growth of thin Si oxide in a cyclic oxygen plasma environment below 200 °C

The growth of Si oxide by means of a cyclic radio-frequency (rf) plasma oxidation process has been explored in a low temperature range of 100-200 °C. The growth mechanism exhibits Cabrera-Mott (CM) oxidation, that is, the transport of mobile ionic species is assisted by an electric field. The low activation energy of 0.3 eV is attributed to the small size of O⁻ and the assistance of the electric field. The oxide becomes off-stoichiometric as one approaches to the exterior surface of the oxide layer.     

Ultraviolet photodissociation at 266 nm of phosphorylated peptide cations

Ultraviolet (UV) photodissociation (PD) experiments using 266 nm light were performed for a series of phosphopeptide cations in a Fourier transform mass spectrometer. The objective of the experiments was to determine whether 266 nm UV irradiation on the phosphopeptide cations would induce unique peptide backbone dissociation. In addition, the general behavior of the phosphate loss (?80 or ?98 Da) was monitored, particularly for those phosphopeptides with a phosphotyrosine residue that itself is a UV chromophore. For phosphopeptides with a UV chromophore, their photodissociation behavior was very similar to that of low‐energy sustained off‐resonance irradiation collisionally activated dissociation (SORI‐CAD), with a few exceptions. For example, b‐ and y‐type peptide backbone fragments were prevalent, and their dephosphorylation behavior was consistent with that of the SORI‐CAD results. For phosphoserine peptides, the loss of a phosphate group was always observed. On the other hand, for phosphotyrosine peptides, the phosphate loss was found to be dependent on the presence of a basic amino group in the sequence and the charge state of the precursor ions, in agreement with the CAD results in the literature. However, hydrogen atom loss or aromatic side chain loss, which is known to be the excited state specific fragmentation pathway, was rarely observed in our 266 nm UV PD experiments, in contrast to the previous UV PD literature (particularly at 220 nm). The mechanism for these observations is described in terms of dominant internal conversion followed by intramolecular vibrational energy redistribution (IVR). Copyright © 2009 John Wiley & Sons, Ltd.