苦瓜中维生素C含量的测定

建立苦瓜中维生素C含量直接测定新方法。以10%盐酸溶液为溶剂,采用紫外分光光度法测定含量。维生素C在0—10μg/mL浓度范围内与吸光度呈良好的线性关系,回归方程为：y=0.04746C＋0.00109,r=0.9997。检出限为0.023μg/mL,加标回收率在94.8%—101.1%之间。该法操作简单,干扰离子少,结果准确,测量快速、准确度和灵敏度高,可应用于维生素C含量的测定。     

Science based calibration for the extraction of 'analyte-specific' HPLC-DAD chromatograms in environmental analysis

Multivariate science based calibration (SBC) has been applied to the resolution of overlapped peaks in liquid chromatography with diode array detection (LC-DAD). Complex river water samples spiked with 11 pharmaceutical substances resulted in poorly resolved chromatograms containing additional peaks from interfering matrix compounds and a change in the background absorbance due to the mobile phase gradient. Applying the present multivariate approach it was possible to resolve all 11 analytes from overlapping peaks, obtaining linear calibration lines (R² > 0.96). Recovery percentages on spiked samples ranged between 74.6 and 113.5%, which are quite satisfactory taking into account the low concentration ranges considered to 1-7 μg L⁻¹.     

A Penning trap for g-factor measurements in highly charged ions by laser-microwave double-resonance spectroscopy

Precise determination of bound-electron g-factors in heavy highly-charged ions (e.g. Bi^82?+?, U^91?+?) provides a stringent test of bound-state QED in extreme fields. With a laser-microwave double-resonance technique we will probe the microwave transitions between the Zeeman sub-levels of the hyperfine structure in highly charged ions. From this the bound electron g-factor g_J can be determined. We present the experimental progress of this novel method to measure the g-factor of the bound electron in highly charged ions.     

Determination of lecithin and soybean oil in dietary supplements using partial least squares-Fourier transform infrared spectroscopy

Lecithin and soybean oil in dietary supplements were determined by Fourier transform infrared spectrometry transmission measurements in dichloromethane in combination with a partial least squares (PLS) regression. Two different PLS models were developed, using 16 synthetic mixtures of analytes in dichloromethane, making measurements in the spectral range from 931.8 to 1252.3 cm⁻¹ for lecithin and from 911.4 to 1246.9 cm⁻¹ and 1695.3 to 1774.5 cm⁻¹ for soybean oil. Seven products from the Spanish market with lecithin concentrations between 21.1% and 99.1% and soybean oil concentrations between 0% and 37.2% were analyzed by the proposed method and the data was compared to a chromatographic reference procedure obtaining accurate results. For samples spiked with amounts between 50 and 250 mg of lecithin and soybean oil recovery percentages between 98.0% and 102.1% and between 93.6% and 102.0% with an average precision of 0.35% and 0.41% were achieved for lecithin and soybean oil, respectively. This method can be applied for the quality control of dietary supplements.     

A REALIZATION OF CERTAIN MODULES FOR THE <Emphasis Type="Italic">N</Emphasis> = 4 SUPERCONFORMAL ALGEBRA AND THE AFFINE LIE ALGEBRA <Emphasis Type="Italic">A</Emphasis><Stack><Subscript>2</Subscript><Superscript>(1)</Superscript></Stack>

We shall first present an explicit realization of the simple N = 4 superconformal vertex algebra L _c ^N?=?4 with central charge c = ?9. This vertex superalgebra is realized inside of the bcβγ system and contains a subalgebra isomorphic to the simple affine vertex algebra L _A1 \( \left(-\frac{3}{2}{\varLambda}_0\right) \). Then we construct a functor from the category of L _c ^N?=?4 -modules with c = ?9 to the category of modules for the admissible affine vertex algebra L _A1 \( \left(-\frac{3}{2}{\varLambda}_0\right) \). By using this construction we construct a family of weight and logarithmic modules for L _c ^N?=?4 and L _A1 \( \left(-\frac{3}{2}{\varLambda}_0\right) \). We also show that a coset subalgebra L _A1 \( \left(-\frac{3}{2}{\varLambda}_0\right) \) is a logarithmic extension of the W(2; 3)-algebra with c = ?10. We discuss some generalizations of our construction based on the extension of affine vertex algebra L _A1 (kΛ ₀) such that k + 2 = 1/p and p is a positive integer.     

Determination of glycolic acid in cosmetics by online liquid chromatography–Fourier transform infrared spectrometry

An isocratic online liquid chromatography Fourier transform infrared procedure has been developed for the determination of glycolic acid in cosmetics. The method involves the ultrasound-assisted extraction of glycolic acid from the samples with an acetonitrile:phosphate buffer (25 mM, pH 2.7) (3:97 v/v). The extracts were centrifuged and filtered before their injection into the chromatography system, which was equipped with a C18 column and used a flow rate of 150 microL min(-1). FTIR spectra were acquired using a time-resolved rapid scan mode. To calculate the chromatograms, the spectral area was integrated between 1288 and 1215 cm(-1), with baseline correction established between 1319 and 1150 cm(-1), after correcting for the eluent spectral background. Peak area values of the extracted sample chromatograms were interpolated from an external calibration curve. The method provided a limit of detection of 0.034 mg mL(-1) and a relative standard deviation of 6% for five measurements at the 0.174 mg mL(-1) concentration level. Recovery values obtained by spiking 400 mg of three commercially available samples with amounts of glycolic acid from 3.7 to 9.8 mg ranged between 99.6 and 101%. The results obtained for the commercial samples agree well with their declared concentrations. An attempt to directly determine glycolic acid by attenuated total reflectance measurements using partial least squares calibration showed that results were strongly influenced by compounds coextracted from the matrix.     

Improved air-stable solid aromatic and heterocyclic zinc reagents by highly selective metalations for negishi cross-couplings

Directed metalation using TMPMgCl?LiCl (TMP=2,2,6,6-tetramethylpiperidide) and subsequent transmetalation with Zn(OPiv)(2) leads to aryl and heteroaryl zinc pivalates. After solvent evaporation, easy-to-handle fine powders are obtained that retain most of their activity (>85?%) when exposed to air for 4?h. They smoothly undergo Negishi cross-couplings, and technical-grade solvents can be used without significant loss of yield.     

Electron emission from photo-excited testosterone in water–ethanol solution

Testosterone (TES; 4-androstene-17β-ol-3-on) is found for the first time to eject electrons from its singlet excited state in water–ethanol solvent mixture. This ability was very recently also observed for 17β-estradiol (17βE2) and progesterone (PRG)/1/. With increasing TES-concentration, the yield of solvated electrons (${\text{e}}_{\text{s}}^{-}$) is decreasing, because of “associate” formation. At higher absorbed UV-doses (λ = 254 nm) the ${\text{e}}_{\text{s}}^{-}$ yield is passing a sharp maximum by formation of TES–ethanol adducts, which are able likewise to emit electrons when excited. At prolonged irradiation the resulting photolytic products of TES–ethanol adducts are also able to emit electrons.The capability of the hormones: 17βE2, PRG and TES to eject electrons and the resulting metabolites, some of which can induce cancer, is discussed.     

MODELLING OF RELEASE OF GAS FROM HIGH-PRESSURE PIPELINES

The problem investigated is the break of a high-pressure pipeline carrying natural single-phase gas which may condensate (retrograde) when the pressure drops. Single-phase non-ideal gas is assumed using a general- ized equation of state. Taking advantage of the choked massflow condition, the break is split into a pipe flow problem and a dispersion flow problem, both solved using a finite difference control volume scheme. The transient flow field from the pipeline break location is expanded analytically, using an approximation of the governing equations, until ambient pressure is reached and matched to the corresponding gas dispersion flow field using as subgrid model a jet box with a time-varying equivalent nozzle area as an internal boundary of the dispersion domain. The turbulence models used for the pipe and dispersion flow fields are an empirical model of Reichard and the k–ϵ model for buoyant flow respectively. The pipe flow simulations indicate that the flow from the pipeline might include dispersed condensate which will affect quantitatively the mass flow rate from the pipeline and qualitatively the gas dispersion if the condensate rains out. The transient dispersion simulation shows that an entrainment flow field develops and mixes supersaturated gas with ambient warmer air to an unsaturated mixture. Because of the inertia of the ambient air, it takes time to develop the entrainment flow field. As a consequence of this and the decay of the mass flow with time, the lower flammability limit of the gas–air mixture reaches its most remote downstream position relatively early in the simulation (about 15 s) and withdraws closer to the break location.