Recebido em 8/4/08; aceito em 14/7/08; publicado na web 5/12/08 THE STATE OF ART OF ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY. Ultra Performance Liquid Chromatography (UPLC) retains the same principles as High Performance Liquid Chromatography (HPLC), but uses 1-2.1 mm i.d. columns with sub-2 µm particles. It is considered the newest advance in analytical separation science. The use of these small particles with mobile phases at high linear velocities increases resolution and detectability and decreases analysis time. Thus, the analyses are faster, the solvent volume is smaller, the efficiency is higher and the detectability is 2-3 times higher when compared with HPLC analysis.

Human milk is related to the physiological and nutritional welfare of newborns, providing the necessary dietary energy, physiologically active compounds and essential nutrients for breastfed babies. Human milk fat has an important position as energy source, structural and regulatory functions, being one of the most important components of breast milk. It provides approximately 50-60% of the energy of the human milk, and its composition in fatty acids defines its nutritional and physico-chemical properties. Furthermore, human milk contains the longchain polyunsaturated essential fatty acids (LCPUFA) eicosapentaenoic acid (EPA), arachidonic acid (AA) and docosahexaenoic acid (DHA), which is important for appropriate development of baby's organs, tissues and nervous system. This chapter will address the benefits associated with the consumption of human milk (health, nutritional, immunological and developmental benefits) as well as the analysis applied to determine the lipid quality of this powerful food.

Recebido em 15/12/09; aceito em 1/4/10; publicado na web em 29/6/10 MODERN STATIONARY PHASES FOR REVERSED PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY. This review first discusses the limitations of many of the supports and stationary phases used in reversed phase high performance liquid chromatography and then describes those, developed more recently, that present better stabilities and more versatile selectivities. Emphases will be given to stationary phases that use higher purity silicas, hybrid silicas, monolithic silicas, metallic oxides and mixed oxides as supports and those that have embedded polar groups or contain phenyl or fluoro groups as the stationary phase as well as the phases used for mixed mode or hydrophilic interaction separations. These modern stationary phases facilitate the analysis of complex mixtures.Keywords: RP-HPLC; modern stationary phases; stability. INTRODUÇÃOO alto nível de desenvolvimento e expansão alcançado pela cromatografia líquida de alta eficiência em fase reversa (CLAE-FR), ao longo das últimas décadas, deve-se principalmente a sua vasta aplicabilidade, que engloba o desenvolvimento de novos produtos, o controle da qualidade desses produtos e, também, as possíveis contaminações provenientes desses produtos e dos disponíveis no mercado há anos. Dentro deste contexto estão envolvidas as indústrias farmacêuticas, alimentícias, agropecuárias e químicas, as agências reguladoras que tratam do meio ambiente e outras. A ampla aplicabilidade da CLAE-FR foi o que impulsionou e continua impulsionando as pesquisas em busca do aprimoramento desta técnica, principalmente referente ao desenvolvimento de novas fases estacionárias (FE). Hoje a CLAE-FR pode ser considerada uma técnica de análise (separação, confirmação e quantificação) bem difundida e empregada, em consequência das colunas cromatográficas e equipamentos de alta tecnologia que se encontram disponíveis.As FE empregadas em CLAE-FR consistem de uma camada orgânica apolar ligada quimicamente ou imobilizada ou apenas sorvida a um suporte cromatográfico. A forma de obtenção dessas camadas apolares e a variedade de óxidos empregados como suportes cromatográficos resultam nos diferentes tipos de FE. O método mais comum e também o mais empregado para a obtenção das FE consiste na introdução de monocamadas orgânicas através de reações com reagentes apropriados, que dá origem às fases estacionárias quimicamente ligadas (FEQL).1-4 As FEQL podem ser obtidas por diferentes processos, como esterificação, cloração seguida por reação com reagente de Grignard ou com compostos organo-lítio e organossilanização. Uma forma alternativa de preparo de FE é o método de recobrimento do suporte com polímeros orgânicos, que pode ser realizado de duas maneiras: mistura de um polímero pré-sintetizado de composição química bem definida em solução com o suporte e posterior evaporação do solvente e, polimerização in situ de uma solução de monômeros ou oligômeros, iniciada ou propagada na superfície do suporte, geralmente seguida de uma etapa de imobilização....

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This study provides a fast, accurate and reproducible method for L-ascorbic acid (L-AA) determination in milk samples by ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). A small volume of a low toxicity organic solvent (ethanol) was used for degreasing and deproteinization steps. Ethylenediaminetetraacetic acid disodium salt (EDTA) and formic acid were used as stabilizing agents. The method was successfully validated in terms of linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and inter/intra-day precision and applied in raw and processed milk samples. Good linearity (r 2 > 0.9915) and low LOD and LOQ, 1.5 and 5.0 µg L-1 , respectively, were obtained. The recoveries for 500 and 1000 µg L-1 spikes were higher than 90% and the precision values expressed in terms of relative standard deviation (RSD) were ≤ 6.8%. For the first time, the determination of L-AA in a 500 µg L-1 concentration range was reported for milk samples.

At the present time, more complex analyses of apolar compounds with similar chemical structures or of polar compounds, especially basic ones, having diverse properties require more selective stationary phases having better stabilities. This paper describes several new stationary phases with directed selectivities that were prepared by immobilizing two different phenyl group-containing siloxanes and a trifluoropropyl-containing siloxane onto chromatographic silica and, in the case of the fluorinated siloxane, onto zirconized silica, using thermal treatment or microware radiation. The chromatographic properties and stabilities of these new phases were determined and several applications were evaluated. The phenyl-containing phases showed excellent characteristics related to the separation of several different types of aromatic compounds while the fluorinated phases, which present a more polar character, revealed selectivity for the separation of positional isomers as well as for a mixture of basic pharmaceuticals. Stability tests indicate that immobilization of the polysiloxanes increases column lifetimes by making the stationary phases less susceptible to dissolution, while the phases immobilized with microwave radiation were somewhat more stable than those immobilized by thermal treatments.

To compare the pharmacokinetics of amoxicillin (AMX) in obese and nonobese subjects, given as single dose 875-mg tablets.Methods: A prospective, single-centre, open-label, clinical study was carried out involving 10 nonobese and 20 obese subjects given a dose of an AMX 875-mg tablet. Serial blood samples were collected between 0 and 8 hours after administration of AMX and plasma levels were quantified by liquid chromatography-tandem mass spectrometry. The pharmacokinetic parameters (PK) were calculated by noncompartmental analysis and means of the 2 groups were compared using Student t-test. Analysis of correlation between covariates and PK was performed using Pearson's correlation coefficient.Results: Ten nonobese subjects (mean age 30.6 ± 7.12 y; body mass index 21.56 ± 1.95 kg/m 2 ) and 20 obese subjects (mean age 34.47 ± 7.03 y; body mass index 33.17 ± 2.38 kg/m 2 ) participated in the study. Both maximum concentration (C max ; 12.12 ± 4.06 vs. 9.66 ± 2.93 mg/L) and area under the curve (AUC) 0-inf (34.18 ± 12.94 mg.h/L vs. 26.88 ± 9.24 mg.h/L) were slightly higher in nonobese than in obese subjects, respectively, but differences were not significant. The volume of distribution (V/F) parameter was statistically significantly higher in obese compared to nonobese patients (44.20 ± 17.85 L vs. 27.57 ± 12.96 L). Statistically significantThe authors confirm that the PI for this paper is Sérgio Seiji Yamada and that he had direct clinical responsibility for the patients.