Characterization and application of a new ultraviolet derivatization reagent for amino acids analysis in capillary electrophoresis

A new ultraviolet (UV) labeling reagent, p-acetamidobenzenesulfonyl fluoride (PAABS-F), was designed and synthesized to label and determine the amino acids by capillary electrophoresis (CE) with diode-array detector (DAD). PAABS-F is very stable and easy to synthesize. It reacted with primary or secondary amino acids very quickly under facile conditions to give corresponding derivatives in high yield with excellent sensitivity and stability. No by-products were observed in amino acid derivatives when stored at room temperature under natural daylight for at least 7 days. Both amino acids standard solution and real samples reacted with this new UV labeling reagent smoothly to form high UV-absorption derivatives. The labeled 20 standard amino acids were efficiently separated by CE and the mass detection limits (S/N = 3) were ranged from 59.3 fmol for l-tryptophan to 1.70 pmol for l-histidine.     

Genetic algorithms (GA) applied to the orthogonal projection approach (OPA) for variable selection

Multivariate curve resolution (MCR) and especially the orthogonal projection approach (OPA) can be applied to spectroscopic data and were proved to be suitable for process monitoring. To improve the quality of the on-line monitoring of batch processes, it is interesting to get as many as possible spectra in a given period of time. Nevertheless, hardware limitations could lead to the fact that it is not possible to acquire more than a certain number of spectra in this given period of time. Wavelength selection could be a good way to limit this problem since it decreases size, and consequently the acquisition time, of each recorded spectrum. This paper details an industrial application of genetic algorithms (GA) coupled with a curve resolution method (OPA) for such purpose.     

基于光纤光参量放大的光脉冲压窄技术的研究

在高重复频率的光窄脉冲源中,为了获得更窄的脉冲,需要增加泵浦功率|但泵浦功率的提高会使光放大器的增益趋于饱和,放大的自发辐射噪音增强,脉冲光信噪比下降.为此,提出了利用啁啾管理和光纤光参量放大相结合的脉冲压窄方案.将强度调制后的泵浦光通过相位调制引入线性负啁啾,由于经参量过程后在新的闲频光上啁啾会加倍,从而进一步增大了信号的谱宽,并通过色散补偿介质实现了光脉冲压缩.实验给出了10 GHz速率下的结果,通过泵浦光的相位调制在0.5 W平均泵浦光功率条件下得到了脉宽19 ps的光脉冲,结果与理论分析基本吻合.     

Bandwidth and stability enhancement of optical parametric amplification using chirped ferroelectric superlattice

We report a theoretical analysis and numerical simulation of bandwidth and stability enhancement in optical parametric amplification (OPA) when using chirped periodically poled KTiOPO₄. Calculation results show that the bandwidth and stability are enhanced significantly by the use of a chirped grating. Temperature-gradient and fanned gratings are introduced and chirp factors of them are deduced and calculated. The use of a fanned grating flattens the Quasi-phase-matching response and improves the efficiency. Finally, we propose a method to reduce the instability induced by an unstable pump.     

Thiosugars--derivatization agents for chiral resolution of homoleucines

o-Phthaldialdehyde was used in combination with a series of six thiosugars for the pre-column chiral derivatization of selected primary amino acids. The diastereomers were resolved on a conventional reversed-phase column and with fluorescence detection. A surprisingly effective resolution of 1-isoindolyl-(1-thioglycosides) derived from 1-thio-beta-L-fucose was observed.     

Femtosecond laser source for real-time atmospheric gas sensing in the UV–visible

We propose an experimental method for detecting molecules in the UV–visible range using ultrashort laser pulses. Two types of sources are used: a continuum generated by 200 kHz Ti:sapphire regenerative amplifier system extending from 320 to 1100 nm, and a near-gaussian femtosecond pulse (100 fs) generated by an optical parametric amplifier. Both broadband sources allow the real-time detection of the oxygen, the nitrogen dioxide NO₂ and the water vapor bands. Moreover, the concentration of NO₂ can be determined within the 10 ppb sensitivity range by using a specific nonlinear fit technique.     

Resolution of overlapped non-absorbing and absorbing solutes using either an absorption null-balance detection window or multivariate deconvolution applied to capillary electrophoresis of anionic surfactants

Non-absorbing alkyl ether sulfates (AES) can be separated using anthraquinone-2-carboxylic acid (AQCA) as a probe; however, absorbing alkyl benzene sulfonates (ABS), if present, interfere indirect detection of most AES oligomers. Overcoming of this interference, as well as the simultaneous characterisation and evaluation of AES, fatty acids and ABS, was accomplished by using a diode-array detector and the procedures here discussed. First, it was shown that ABS can be made undetectable by using a 9 nm wide and 227 nm centred charge-absorptivity null-balance detection window (NBDW), where its contribution to the absorbance cancels the dilution effects that its presence induces on the signal of the background chromophore (BGC). Two other procedures, not requiring any prior knowledge on the nature of the absorbing interference, were also addressed. In the first one, the NBDW procedure was emulated by software, by treating the time-wavelength data matrix stored during the experimental run, and in the second one, both the ABS and BGC spectra, and the concentration profiles of ABS and the non-absorbing solutes, were recovered by orthogonal projection approach (OPA) and alternating least squares (ALS). The OPA-ALS processing provided the deconvolved signals and the wavelengths required to implement the experimental and software-emulated NBDW procedures. A composite ABS spectrum and a mixed concentration profile of the non-absorbing solutes, that involves mutual ABS-BGC dilution effects are enclosed in the OPA-ALS straightforward solutions. The pure spectra and concentration profiles were finally retrieved by crossed orthogonalisation. For the NBDW procedures, the limits of detection (S/N = 3) for AES oligomers overlapped by 1500 microg ml(-1) ABS were of ca. 10 microM AES. Using decyl sulfate as internal standard, the relative standard deviation for AES in an ABS containing industrial sample was 4.5%. The procedures here described are useful to remove the interference produced by any absorbing solute when overlapped with indirectly detected solutes in both capillary electrophoresis (CE) and HPLC.     

柱后衍生-高效液相色谱法测定玉米中伏马菌素B1和B2

建立了邻苯二甲醛(OPA)柱后衍生-高效液相色谱测定玉米中伏马菌素B1和B2(FB1和FB2)的方法。采用ZORBAX SB-C18色谱柱,以0.1 mol/L磷酸二氢钠溶液(pH 3.3)-甲醇为流动相,梯度洗脱。流动相流速为0.8 mL/min,柱温40 ℃;衍生剂的流速为0.4 mL/min,衍生温度为室温。实验对衍生剂缓冲液的pH、衍生剂的浓度和流速、激发和发射波长等重要条件进行了优化。结果表明,衍生剂的pH在10.5、OPA的质量浓度为2 g/L、流速为0.4 mL/min、激发波长335 nm、发射波长440 nm时测定效果良好,FB1、FB2在0.2～20 mg/L范围内线性关系良好,相关系数大于0.999; FB1和FB2的检出限均为0.02 mg/kg;在0.1～ 4.0 mg/kg范围内,3个添加水平的平均回收率为82.5%～89.8%。该方法精确、简单、快速,适合玉米中FB1和FB2的测定。     

基于光纤光参量放大的光脉冲压窄技术的研究

在高重复频率的光窄脉冲源中,为了获得更窄的脉冲,需要增加泵浦功率;但泵浦功率的提高会使光放大器的增益趋于饱和,放大的自发辐射噪音增强,脉冲光信噪比下降.为此,提出了利用啁啾管理和光纤光参量放大相结合的脉冲压窄方案.将强度调制后的泵浦光通过相位调制引入线性负啁啾,由于经参量过程后在新的闲频光上啁啾会加倍,从而进一步增大了...     

Validation of an ultra high pressure liquid chromatographic method for the determination of biologically active amines in food

Biologically active amines include the so called biogenic amines, such as histamine, tyramine and cadaverine, and polyamines such as spermidine and spermine. Ultra high pressure liquid chromatography (UHPLC) is a new generation of separation techniques that takes full advantage of chromatographic principles to increase speed flow which drastically reduce analysis time. The aim of the present work was to validate a rapid method of UHPLC to detect the presence of biogenic amines and polyamines in food. Different food matrixes (wine, fish, cheese, and dry fermented sausage) were used in order to test the versatility of the method. The UHPLC method described in this article has been demonstrated as a reliable procedure to determine 12 biogenic amines and polyamines in less than 7 min of chromatographic elution. The method provides a satisfactory linearity and chromatographic sensitivity with a detection limit lower than 0.2 mg/L and a determination limit falling below 0.3 mg/L for all amines. The precision, in terms of relative standard deviation, was lower than 5% and the accuracy, as mean recovery, was between 93% and 98%, depending on the food matrix.