高效液相色谱-飞行时间质谱联用法分析人参及人参皂苷与山楂配伍过程中的水解行为

利用高效液相色谱-飞行时间质谱联用的方法,分别对人参配伍山楂前后人参皂苷的变化进行分析,同时对人参皂苷Re、Rg1、Rb1、Rd与山楂配伍的水解规律进行系统研究,并与单独煎煮液、仿山楂配伍pH值煎煮液的水解产物进行比较,结果发现人参与山楂配伍后人参皂苷Rg1、Rb1含量明显减少,而人参皂苷Re、Rd、Rg2、Rg3、F2、Rh1含量明显增加,其中人参皂苷Re与山楂配伍后水解产物为人参皂苷20(R)-Rg2、20(S)-Rg2,仿山楂配伍pH值水解产物为人参皂苷20(R)-Rg2、20(S)-Rg2、Rg4、Rg6;人参皂苷Rg1与山楂配伍后水解产物为20(S)-Rh1、20(R)-Rh1,仿山楂pH值水解产物为20(S)-Rh1、20(R)-Rh1、Rh4、Rk3;人参皂苷Rb1与山楂配伍后水解产物为Rd、20(S)-Rg3,仿山楂pH值水解产物为F2、20(S)-Rg3;人参皂苷Rd与山楂配伍后水解产物为F2、20(S)-Rg3、20(R)-Rg3,仿山楂pH值水解产物为20(S)-Rg3、20(R)-Rg3。研究表明,不同人参皂苷和山楂配伍后与仿山楂pH值的水解产物并不相同,人参与山楂配伍改变了人参皂苷成分的种类及含量。本研究为临床方剂中人参与山楂配伍后成分的变化提供物质基础数据。     

Tissue distribution and excretion study of neopanaxadiol in rats by ultra‐performance liquid chromatography quadrupole time‐of‐flight mass spectrometry

Neopanaxadiol (NPD), a major ginsenoside in Panax ginseng C. A. Meyer (Araliaceae), was reported to have neuroprotective effect. In this study, a method of ultra‐performance liquid chromatography quadrupole time‐of‐flight mass spectrometry (UPLC/QTOF‐MS) was developed and validated for quantitative analysis of NPD in tissues, urine and feces, using liquid–liquid extraction (LLE) to isolate NPD from different biological samples, and chromatographic separation was performed on an Agilent Zorbax Stable Bond C₁₈ (2.1 × 50 mm, 1.8 µm) column with 0.1% formic acid in water and acetonitrile. All standard calibration curves were linear (all r² > 0.995) within the test range. After oral administration, NPD was extensively distributed to most of the tissues without long‐term accumulation. The higher levels were observed in stomach and intestine, followed by kidney and liver. Approximately 64.56 ± 20.32% of administered dose in feces and 0.0233 ± 0.0356% in urine were found within 96 h, which indicated that the major elimination route was fecal excretion. This analytical method was applied to the study of NPD distribution and excretion in rats after oral intake for the first time. The results we found here are helpful for us to understand the pharmacological effects of NPD, as well as its toxicity. Copyright © 2014 John Wiley & Sons, Ltd.     

Determination of pseudo‐ginsenoside GQ in human plasma by high performance liquid chromatography–tandem mass spectrometry

A specific, sensitive and rapid method based on high performance liquid chromatography coupled to tandem mass spectrometry (HPLC‐MS/MS) was developed for the determination of pseudo‐ginsenoside GQ in human plasma. Liquid–liquid extraction was used to isolate the analyte from biological matrix followed by injection of the extracts onto a C₈ column with isocratic elution. Detection was carried out on a triple quadrupole tandem mass spectrometer (API‐4000 system) in multiple reaction monitoring mode using negative electrospray ionization. The mobile phase consisted of methanol–10 mm ammonium acetate (90:10, v/v) and the flow rate was 0.3 mL/min. The method was validated over the concentration range of 5.0–5000.0 ng/mL for plasma. Inter‐ and intra‐day precisions (relative standard deviation) were all within 15% and the accuracy (relative error) was ≤9.4%. The lower limit of quantitation was 5.0 ng/mL. The pseudo‐ginsenoside GQ was stable after 8 h at room temperature, 24 h at autosampler and three freeze–thaw cycles (from ?30 to 25 °C). The method was successfully applied to the pharmacokinetic study of pseudo‐ginsenoside GQ in healthy Chinese volunteers. Copyright © 2013 John Wiley & Sons, Ltd.     

固相萃取-超高效液相色谱法测定人参中5种原人参二醇型人参皂苷的含量

建立了固相萃取-超高效液相色谱测定人参中5种原人参二醇型人参皂苷的方法。人参药材经粉碎后通过水饱和正丁醇溶液进行超声提取,经过亲水作用固相萃取柱净化后,在ACQUITY UPLC BEH Shield RP18色谱柱（100 mm×2.1 mm,1.7 μm）上分离,利用乙腈/水作为流动相进行梯度洗脱,采用光电二极管阵列检测器检测。结果表明,5种原人参二醇型人参皂苷在5~500 μg/mL范围内具有很好的线性关系,相关系数均大于0.999。方法精密度的RSD值在0.95%~2.62%（n=6）之间,22 h内样品稳定性的RSD值在0.90%~2.15%（n=8）之间,日内和日间重复性的RSD值分别为5.35%~6.47%（n=6）和5.56%~6.34%（n=8）。方法的加标回收率在87.16%~101.92%之间,相对标准偏差在1.54%~4.01%（n=6）之间。所建立的方法采用亲水作用色谱模式的固相萃取材料,药材的提取液可直接作为固相萃取的上样溶液进行人参皂苷的富集和净化,并且超高效液相色谱大大缩短了分析时间。该方法简单快速、通量高、重现性好,适用于人参中5种原人参二醇型人参皂苷的定量分析。     

Renormalization group dependence of the QCD coupling

The general relation between the standard expansion coefficients and the beta function for the QCD coupling is exactly derived in a mathematically strict way. It is accordingly found that an infinite number of logarithmic terms are lost in the standard expansion with a finite order, and these lost terms can be given in a closed form. Numerical calculations, by a new matching-invariant coupling with the corresponding beta function to four-loop level, show that the new expansion converges much faster.     

超声辅助结合离子液体双水相提取-高效液相色谱法测定三七中5种稀有人参皂苷的含量

建立了超声辅助结合离子液体双水相提取-高效液相色谱法测定三七中5种稀有人参皂苷20(S)-Rg_2,20(S)-Rh_1,Rk_3,20(S)-Rg_3及Rk_1含量的方法.考察了影响提取率的多种因素并确立了最佳提取条件,在该条件下,5种稀有人参皂苷加样回收率均在92.07%~110.55%之间,RSD值均5.43%.实验结果表明,该方法具有快速、高效、准确且环保等优点,为中药材及其制剂中微量化学成分的提取、富集与分析提供了参考.     

Direct construction of the effective action of chiral gauge fermions in the anomalous sector

The anomaly implies an obstruction to a fully chiral covariant calculation of the effective action in the abnormal-parity sector of chiral theories. The standard approach then is to reconstruct the anomalous effective action from its covariant current. In this work, we use a recently introduced formulation which allows one to directly construct the non-trivial chiral invariant part of the effective action within a fully covariant formalism. To this end we develop an appropriate version of Chan’s approach to carry out the calculation within the derivative expansion. The result to four derivatives, i.e., to leading order in two and four dimensions and next-to-leading order in two dimensions, is explicitly worked out. Fairly compact expressions are found for these terms.     

Gain versus tuning issues to Q-switch with Yb<Superscript>3+</Superscript>:LSO and amplify broad-bandwidth pulses

We report on the development of Incoherent Broadband Cavity Enhanced Absorption Spectroscopy (IBBCEAS) using a blue light emitting diode (LED) for the detection of NO₂ in laboratory ambient air. Absorption of the oxygen collisional pair in the atmosphere was also detected in the same spectral range. The mirror reflectivity was determined using a standard gas sample mixture of NO₂, and calibrated with the help of the absorption spectrum of the oxygen collisional pair in pure oxygen at atmospheric pressure. Optimization of the experimental parameters was investigated and is discussed in detail. For the first time in IBBCEAS involving broadband absorption spectra, averaging time for signal-to-noise ratio enhancement has been optimized using Allan variance plot. 18.1 ppbv NO₂ in laboratory ambient air has been retrieved from the absorption spectra using differential fitting method over a 40 nm spectral region centered at 470 nm. A minimum detection sensitivity of about 2.2 ppbv (1σ) for NO₂ at atmospheric pressure has been achieved using the optimal averaging time of 100 s by means of a high finesse optical cavity formed with two moderate reflectivity (∼99.55%) mirrors. No purging of the cavity mirrors by high purity He or N₂ gas streams was necessary to prevent contamination of the mirror faces for the in situ measurements.     

Perturbative chiral violations for domain-wall QCD with improved gauge actions

We investigate, in the framework of perturbation theory at finite Ns$N_s$, the effectiveness of improved gauge actions in suppressing the chiral violations of domain-wall fermions. Our calculations show substantial reductions of the residual mass when it is compared at the same value of the gauge coupling, the largest suppression being obtained when the DBW2 action is used. Similar effects can also be observed for a power-divergent mixing coefficient which is chirally suppressed. No significant reduction instead can be seen in the case of the difference between the vector and axial-vector renormalization constants when improved gauge actions are used in place of the plaquette action. We also find that one-loop perturbation theory is not an adequate tool to carry out comparisons at the same energy scale (of about 2 GeV), and in fact in this case even an enhancement of the chiral violations is frequently obtained.     

UA(1) anomaly and $ \eta^{{\prime}}_{}$ -mass from an infrared singular quark-gluon vertex

The U _A(1) problem of QCD is inevitably tied to the infrared behaviour of quarks and gluons with its most visible effect being the -mass. A dimensional argument of Kogut and Susskind showed that the mixing of the pseudoscalar flavour-singlet mesons with gluons can provide a screening of the Goldstone pole in this channel if the full quark-quark interaction is strongly infrared singular as ∼ 1/k ⁴ . We investigate this idea using previously obtained results for the Landau gauge ghost and gluon propagator, together with recent determinations for the singular behaviour of the quark-gluon vertex. We find that, even with an infrared vanishing gluon propagator, the singular structure of the quark-gluon vertex for certain kinematics is apposite for yielding a non-zero screening mass.