HPLC与MALDI-TOFMS联用技术分析蛋黄中的磷脂

蛋黄中含有大量磷脂,其中磷脂酰胆碱(PC)和磷脂酰乙醇胺(PE)最为丰富。本研究采用高效液相色谱法(HPLC)与基质辅助激光解吸电离飞行时间质谱(MALDI-TOF MS)联用技术分析了蛋黄中磷脂粗提物。将从蛋黄中提取的多种磷脂通过HPLC预先分离,收集各组分后分别进行MALDI-TOF MS分析得到比较清晰的质谱图。通过质谱图解析确定了蛋黄中磷脂酰胆碱、神经鞘磷脂(SM)的脂肪酸组成。

UV-B辐射增强对长白山五种藓类植物生长的影响

对生长在中国长白山的5种藓类植物——垂枝藓、拟垂枝藓、塔藓、星塔藓和高山金发藓分别以辐射强度为0.2(自然光照,对照)、3.0(紫外线中等辐射强度)和6.0kJ.m-2.d-1(高剂量辐射强度)的UV-B照射40d后,测定其株高、生物量及叶绿素含量.结果表明:中等和高强度的UV-B辐射使拟垂枝藓和塔藓的株高、生物量和叶绿素含量分别下降了32.3%、62.4%、81.3%和21.4%、59.4%、62.8%,其相对生长速率均为负值;高剂量UV-B辐射处理下垂枝藓的生物量稍有上升,而高山金发藓地下部分的生物量增加1倍,但叶绿素含量变化不明显.高山金发藓和垂枝藓抵抗UV-B辐射的能力较强,拟垂枝藓和塔藓对UV-B辐射较敏感.

UV-B增强对番茄的伤害及H_2O_2的防护作用

UVB辐射使番茄叶片的叶绿素a,叶绿素b及总叶绿素含量先升高后降低,同样使叶片的抗氧化酶过氧化氢酶(CAT)和过氧化物酶(POD)活性先升高随后降低,而使超氧化物歧化酶(SOD)活性升高,膜脂过氧化产物MDA的含量增加;中等剂量(5mmol·l-1)的H2O2预处理能提高叶绿素b的含量,明显提高抗氧化酶的活性,并延缓CAT活性的降低,抑制膜质过氧化产物MDA的产生.中等浓度H2O2预处理能提高番茄对UVB增强的抗性.

Determination and identification of isoflavonoids in Radix astragali by matrix solid-phase dispersion extraction and high-performance liquid chromatography with photodiode array and mass spectrometric detection

The isoflavonoids in Radix astragali were determined and identified by HPLC-photodiode array detection-MS after extraction employing matrix solid-phase dispersion (MSPD). As a new sample preparation method for R. astragali, the MSPD procedure was optimized, validated and compared with conventional methods including ultrasonic and Soxhlet extraction. The amounts of two major components in this herb, formononetin (6) and ononin (2), were determined based on their authentic standards. Four major isoflavonoids, formononetin (6), ononin (2), calycosin (5) and its glycoside (1), and three minor isoflavonoids, (6aR,11aR)-3-hydroxy-9, 10-dimethoxypterocarpan (7), its glycoside (3), and (3R)-7,2'-dihydroxy-3',4'-dimethoxyisoflavone-7-O-beta-D-glycoside (4), were identified based on their characteristic two-band UV spectra and [M + H](+), [aglycone + H](+) and [A1 + H](+) ions, etc. The combined MSPD and HPLC-DAD-MS method was suitable for quantitative and qualitative determination of the isoflavonoids in R. astragali. (C) 2003 Elsevier B.V. All rights reserved.

不同UV-C辐射时间对豌豆幼苗光合特性及抗氧化酶活性的影响

研究了不同UV-C辐射时间对豌豆幼苗光合特性及抗氧化酶活性的影响。结果表明,UV-C辐射增强使叶片光合速率减弱,气孔导度、胞间CO2浓度、蒸腾速率和羧化效率明显降低,CO2补偿点升高。随着UV-C辐射时间的延长,POD和CAT活性先升高随后降低,SOD活性、叶绿素含量则逐渐降低,但丙二醛含量逐渐增加。这说明UV-C辐射增强引起抗氧化酶活性降低,使膜脂过氧化,导致光合作用减弱。

Using HPLC retention parameters to estimate fish bioconcentration factors of organic compounds

Reversed-phase high performance liquid chromatography (RP-HPLC) was employed to develop predictive models for fish bioconcentration factors (BCF) of organic compounds. Estimation of BCF from RP-HPLC retention parameters on octadecyl-bonded silica gel (ODS), cyanopropyl-bonded silica gel (CN), and phenyl-bonded silica gel (Ph) columns were investigated. The results show that, for a set of compounds belonging to different chemical classes, the CN stationary phase is the best one among the three columns and better than n-octanol/water model for BCF estimation. A multi-column RP-HPLC model, using the retention parameters on the CN and Ph columns as the variables of multiple linear regression equations, was further evaluated to estimate BCF of organic compounds belonging to different chemical classes, and the results show that the multi-column RP-HPLC model is better than that of any single RP-HPLC column for BCF estimation.

Study of an electroosmotic pump for liquid delivery and its application in capillary column liquid chromatography

A packed-bed electroosmotic pump (EOP) was constructed and evaluated. The EOP consisted of three capillary columns packed in parallel, a gas-releasing device, Pt electrodes and a high-voltage power supply. The EOP could generate output pressure above 5.0 MPa and constant flow rate in the range of nl/min to a few mul/min for pure water, pure methanol, 2 mM potassium dihydrogenphosphate buffer, the buffer-methanol mixture and the pure water-methanol mixture at applied potentials less than 20 W The composition of solvent before/after pumping was quantitatively determined by using a gas chromatograph equipped with both flame ionization detector and thermal conductivity detector. It was found that there were no apparent changes in composition and relative concentrations after pumping process for a methanol-ethanol-acetonitrile mixture and a methanol-water mixture. Theoretical aspect of the EOP was discussed in detail. An capillary HPLC system consisting of the EOP, an injection valve, a 15 cm x 320 mum i.d., 5 mum Spherigel C(18) stainless steel analytical column, and an on-column UV detector was connected to evaluate the performance of the EOP. A comparative study was also carried out with a mechanical capillary HPLC pump on the same system. The results demonstrated that the reproducibility of flow rate and the pulsation-free flow property of the EOP are superior to that of mechanical pump in capillary HPLC application. (C) 2004 Elsevier B.V. All rights reserved.

Retention modeling and simultaneous optimization of pH value and gradient steepness in RP-HPLC using feed-forward neural networks

A novel approach is proposed for the simultaneous optimization of mobile phase pH and gradient steepness in RP-HPLC using artificial neural networks. By presetting the initial and final concentration of the organic solvent, a limited number of experiments with different gradient time and pH value of mobile phase are arranged in the two-dimensional space of mobile phase parameters. The retention behavior of each solute is modeled using an individual artificial neural network. An "early stopping" strategy is adopted to ensure the predicting capability of neural networks. The trained neural networks can be used to predict the retention time of solutes under arbitrary mobile phase conditions in the optimization region. Finally, the optimal separation conditions can be found according to a global resolution function. The effectiveness of this method is validated by optimization of separation conditions for amino acids derivatised by a new fluorescent reagent.