high performance liquid chromatography

高效液相色谱法
  • 文章类型: Journal Article
    在这项研究中,介绍了有关橄榄果实中几种生物活性化合物测定的总体调查。开发了两种方法,一种用于测定橄榄果实酚类化合物的UPLC-Q-TOF-MS方法和一种针对色素(叶绿素和类胡萝卜素)测定的HPLC-DAD方法,生育酚(α-,β,-γ,δ-)和角鲨烯。开发了目标和可疑筛查工作流程,以对橄榄的酚类成分进行彻底的指纹识别。两种方法都得到了验证,表现出优异的性能特点,并且可以用作监测橄榄果实样品中生物活性化合物的可靠工具。开发的方法用于化学表征科洛维橄榄品种的果实,起源于莱斯沃斯岛,北爱琴海地区,希腊。用天花苷在Kolovi橄榄中鉴定并定量了25种酚类化合物,羟基酪醇,油精和油分浓度很高。此外,使用内部可疑数据库在样品中鉴定了12种新的生物活性化合物。色素分析结果表明,Kolovi品种应具有低色素沉着的特征,与其他橄榄品种相比,生育酚和角鲨烯含量相对较高。Kolovi橄榄生物活性含量的表征强调了Kolovi橄榄果实的高营养和可能的经济价值。
    In this study, an overall survey regarding the determination of several bioactive compounds in olive fruit is presented. Two methodologies were developed, one UPLC-Q-TOF-MS method for the determination of olive fruit phenolic compounds and one HPLC-DAD methodology targeting the determination of pigments (chlorophylls and carotenoids), tocopherols (α-, β, -γ, δ-) and squalene. Target and suspect screening workflows were developed for the thorough fingerprinting of the phenolic fraction of olives. Both methods were validated, presenting excellent performance characteristics, and can be used as reliable tools for the monitoring of bioactive compounds in olive fruit samples. The developed methodologies were utilized to chemical characterize the fruits of the Kolovi olive variety, originating from the island of Lesvos, North Aegean Region, Greece. Twenty-five phenolic compounds were identified and quantified in Kolovi olives with verbascoside, hydroxytyrosol, oleacein and oleomissional found in significantly high concentrations. Moreover, 12 new bioactive compounds were identified in the samples using an in-house suspect database. The results of pigments analysis suggested that Kolovi variety should be characterized as low pigmentation, while the tocopherol and squalene content was relatively high compared to other olive varieties. The characterization of Kolovi olive bioactive content highlighted the high nutritional and possible economic value of the Kolovi olive fruit.
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  • 文章类型: Journal Article
    A high-performance liquid chromatographic method with a modified QuEChERS extraction for the determination of polycyclic aromatic hydrocarbons (PAHs) in blood serum was developed to investigate the internal exposure level and the carcinogentic toxicity contribution rate of PAHs for pregnant women in Nantong, China. Venous blood (n = 48) was collected in the local hospital and the internal exposure level of 16 PAHs and the contribution rate of carcinogenicity to pregnant women were analyzed. Among all of the detected PAHs, the detection rate of pyrene (77.08%) was the highest, followed by naphthalene (64.58%) and benzo[a]anthracene (BaA, 45.83%). The carcinogenicity contribution rate of BaA (37.37%) was the highest, followed by fluorene (32.96%) and acenaphthylene (22.01%). The results showed that many kinds of carcinogenic PAHs can be detected in the serum of pregnant women in Nantong city, among which BaA should be paid most attention because of its high internal exposure level and carcinogenic risk. Meanwhile, the origins of general PAHs in serum samples were analyzed using the characteristic ratio analysis method. The PAH pollution level of air samples (n = 42) during the collection time of blood samples was also analyzed to compare the possible correlations between the two different results.
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  • 文章类型: Journal Article
    High performance liquid chromatography-ultraviolet(HPLC-UV) fingerprint is one of the most important methods for the quality control of Chinese medicines in Chinese Pharmacopoeia. However, certain subjectivity is present in selection of specific band of UV, and the inherent quality differences of Chinese medicine can\'t be well characterized by this method. Therefore, with different grades of Scrophulariae Radix were taken as the research object in this study, a new quality control model of HPLC-UV was established in this study based on the ultraviolet full-wavelength scanning spectrum. Firstly, different grades of Scrophulariae Radix samples were collected, and the full-wavelength ultraviolet absorption spectra of all the samples were established at the bands of 200-400 nm. In order to analyze the differences among samples, the analysis model was built following multivariate statistical analysis methods such as principal component analysis(PCA) and partial least squares discrimination analysis(PLS-DA) after the pretreatment of spectral data. The result showed that the ultraviolet band at 251 nm may contribute most to distinguish the quality differences among different grades of samples. Then, the HPLC fingerprints of samples were established with the band at 251 nm. The multivariate statistical analysis showed that there was a more significant classification trend in HPLC fingerprints than that in the original UV fingerprints, which could be used to distinguish different grades of samples, and could better reflect the differences among different grades. The method reported in this study can be of a great guidance and reference for the establishment of specific fingerprints of Chinese medicines as well as for the quality control of Chinese medicine.
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  • 文章类型: Journal Article
    麻痹性贝类中毒(PSP)的临床病例在阿拉斯加很常见,并且是由于人类食用被沙克霉素(STX)及其类似物污染的贝类。PSP的诊断是推定的,基于最近摄入贝类和存在与PSP症状一致的表现;通过在临床标本或食物样本中检测麻痹性贝类毒素来确认诊断。采用高效液相色谱-串联质谱(HPLC-MS/MS)的临床诊断分析方法,使用2010年6月至2011年11月收集的尿液标本,对11名阿拉斯加患者的蛇毒毒素诱导PSP(STX-PSP)进行了评估。根据肌酐浓度校正尿STX的浓度,以说明来自水摄入或限制的尿液稀释或浓度。分别。在11名疑似PSP患者中,4例患者通过尿液检测(24-364ngSTX/g肌酐)证实患有STX-PSP.尽管5例患者的尿液中未检测到STX,但仍有PSP的临床表现。根据未检测到的尿液STX和没有临床发现,两名患者被排除STX-PSP。结果显示,吞咽困难和构音障碍可能是PSP比感觉异常和恶心更强的指标,通常用于临床诊断PSP患者。PSP也可以通过暴露于许多STX同源物而发生,如gonyautoxins,然而,在这项调查中没有评估它们在尿液中的存在。此外,使用官方分析化学家协会的小鼠生物测定法分析了从六个假定的PSP病例中获得的膳食残留物。所有六个样品的PSP毒素测试为阳性。在未来,临床诊断方法可以与小鼠生物测定法或HPLC-MS/MS结合使用,以评估阿拉斯加STX-PSP的程度,在阿拉斯加,有人建议PSP被低估.
    Clinical cases of paralytic shellfish poisoning (PSP) are common in Alaska, and result from human consumption of shellfish contaminated with saxitoxin (STX) and its analogues. Diagnosis of PSP is presumptive and based on recent ingestion of shellfish and presence of manifestations consistent with symptoms of PSP; diagnosis is confirmed by detection of paralytic shellfish toxins in a clinical specimen or food sample. A clinical diagnostic analytical method using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was used to evaluate the diagnosis of saxitoxin-induced PSP (STX-PSP) in 11 Alaskan patients using urine specimens collected between June 2010 and November 2011. Concentrations of urinary STX were corrected for creatinine concentrations to account for dilution or concentration of urine from water intake or restriction, respectively. Of the 11 patients with suspected PSP, four patients were confirmed to have STX-PSP by urine testing (24-364ng STX/g creatinine). Five patients had clinical manifestations of PSP though no STX was detected in their urine. Two patients were ruled out for STX-PSP based on non-detected urinary STX and the absence of clinical findings. Results revealed that dysphagia and dysarthria may be stronger indicators of PSP than paresthesia and nausea, which are commonly used to clinically diagnose patients with PSP. PSP can also occur from exposure to a number of STX congeners, such as gonyautoxins, however their presence in urine was not assessed in this investigation. In addition, meal remnants obtained from six presumptive PSP cases were analyzed using the Association of Official Analytical Chemists\' mouse bioassay. All six samples tested positive for PSP toxins. In the future, the clinical diagnostic method can be used in conjunction with the mouse bioassay or HPLC-MS/MS to assess the extent of STX-PSP in Alaska where it has been suggested that PSP is underreported.
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  • 文章类型: Journal Article
    The purpose of this study was to examine the possible links between type 2 diabetes, daytime sleepiness, sleep quality and caffeine consumption.
    In this case-control field study, comparing type 2 diabetic ( n=134) and non-type 2 diabetic ( n=230) participants, subjects completed detailed and validated questionnaires to assess demographic status, health, daytime sleepiness, sleep quality and timing, diurnal preference, mistimed circadian rhythms and habitual caffeine intake. All participants gave saliva under standardised conditions for CYP1A2 genotyping and quantification of caffeine concentration. Hierarchical linear regression analyses examined whether type 2 diabetes status was associated with caffeine consumption.
    Type 2 diabetic participants reported greater daytime sleepiness ( p=0.001), a higher prevalence of sleep apnoea ( p=0.005) and napping ( p=0.008), and greater habitual caffeine intake ( p<0.001), derived from the consumption of an extra cup of coffee each day. This finding was confirmed by higher saliva caffeine concentration at bedtime ( p=0.01). Multiple regression analyses revealed that type 2 diabetes status was associated with higher self-reported caffeine consumption ( p<0.02) and higher salivary caffeine ( p<0.02). Next to male sex, type 2 diabetes status was the strongest predictor of caffeine intake. Subjective sleep and circadian estimates were similar between case and control groups.
    Type 2 diabetic patients may self-medicate with caffeine to alleviate daytime sleepiness. High caffeine intake reflects a lifestyle factor that may be considered when promoting type 2 diabetes management.
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  • 文章类型: Case Reports
    先天性糖基化障碍(CDG)是越来越多的遗传性代谢障碍,其中糖脂和/或糖蛋白的形成或加工中的酶缺陷导致多种不同的疾病。GDP-Man的缺乏:GlcNAc2-PP-dolichol甘露糖基转移酶,由来自酵母的ALG1的人类直系同源物编码,被称为ALG1-CDG(CDG-Ik)。表型,1例严重影响的ALG1-CDG患者的分子和生化分析是本文的重点。病人的主要症状是喂养问题和腹泻,深度低蛋白血症伴有大量腹水,肌张力增高,难以治疗的癫痫发作,反复发作的呼吸暂停,心脏和肝脏受累和凝血异常。在患者的ALG1编码序列中检测到突变c.1145T>C(M382T)和c.1312C>T(R438W)的复合杂合性。与先前报道的对R438W的推测相反,我们证实了这两种突变在ALG1-CDG中是致病的。
    Congenital disorders of glycosylation (CDG) are a growing group of inherited metabolic disorders where enzymatic defects in the formation or processing of glycolipids and/or glycoproteins lead to variety of different diseases. The deficiency of GDP-Man:GlcNAc2-PP-dolichol mannosyltransferase, encoded by the human ortholog of ALG1 from yeast, is known as ALG1-CDG (CDG-Ik). The phenotypical, molecular and biochemical analysis of a severely affected ALG1-CDG patient is the focus of this paper. The patient\'s main symptoms were feeding problems and diarrhea, profound hypoproteinemia with massive ascites, muscular hypertonia, seizures refractory to treatment, recurrent episodes of apnoea, cardiac and hepatic involvement and coagulation anomalies. Compound heterozygosity for the mutations c.1145T>C (M382T) and c.1312C>T (R438W) was detected in the patient\'s ALG1-coding sequence. In contrast to a previously reported speculation on R438W we confirmed both mutations as disease-causing in ALG1-CDG.
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