高效液相色谱法同时测定沙枣果实中5种酚类化合物

建立了高效液相色谱法检测沙枣果实中绿原酸、咖啡酸、香豆酸、肉桂酸和阿魏酸等5种酚类物质的方法。样品用乙腈超声提取,色谱柱为HypersilODS100mm×4.6mm（i.d）,5μm柱;流动相为乙腈和磷酸缓冲液（0.6%）,梯度洗脱;流速为1mL/min;检测波长为323nm和280nm;进样量为10μL。5种组分在一定范围内有良好的线性关系,相关系数为0.991～0.997,平均回收率为93.3%～98.1%,相对标准偏差为3.1%～7.4%（n=6）。结果表明：沙枣果实中绿原酸、咖啡酸、香豆酸、阿魏酸和肉桂酸的含量分别为0.472、0.373、0.425、0.529、0.381mg/kg。     

High performance liquid chromatography analysis of anthocyanins in bilberries (Vaccinium myrtillus L.), blueberries (Vaccinium corymbosum L.), and corresponding juices

In the present study the anthocyanin content of commercially available bilberry juices and fresh fruits were quantified by using 15 authentic anthocyanin standards via high performance liquid chromatography with an ultra-violet detector (HPLC-UV/VIS). Delphinidin-3-O-glucopyranoside, delphinidin-3-O-galactopyranoside, and cyanidin-3-O-arabinopyranoside were the major anthocyanins found in juices, nectar, and fresh bilberries. In contrast, fresh blueberries had higher concentrations of malvidin-3-O-arabinopyranoside and petunidin-3-O-galactopyranoside. Up to 438 mg anthocyanins per 100 g fresh weight (2762 mg/100 g dry weight (DW)) were detected in blueberries from various sources, whereas bilberries contained a maximum of 1017 mg anthocyanins per 100 g fresh weight (7465 mg/100 g DW). Commercially available bilberry and blueberry juices (n= 9) as well as nectars (n= 4) were also analyzed. Anthocyanin concentrations of juices (1610 mg/L to 5963 mg/L) and nectar from bilberries (656 mg/L to 1529 mg/L) were higher than those of blueberry juices (417 mg/L) and nectar (258 mg/L to 386 mg/L). We conclude that using several authentic anthocyanin references to quantify anthocyanin contents indicated them to be up to 53% and 64% higher in fresh bilberries and blueberries, respectively, than previously reported using cyanidin-3-O-glucoside. This study has also demonstrated that commercially available juices produced from bilberries contain much higher anthocyanin concentrations than those from blueberries. PRACTICAL APPLICATION: We have investigated the contents of a special class of antioxidants, namely anthocyanins in blueberry and billberry fruits and juices commercially available in Germany. To achieve reliable data we have used authentic standards for the first time. We think that our results are important in the field of nutritional intake of this important class of polyphenols and fruit juice companies get a closer insight in the occurrence of these antioxidants in market samples to be used in food composition databases and for nutritional survey.     

Free amino acids and biogenic amines in Alicante Monastrell wines

The simultaneous determination of 17 free amino acids and 8 biogenic amines in Alicante Monastrell wines was investigated for the first time. The quantification was carried out by using a RP-HPLC method, based on a pre-column derivatization with o-phthaldialdehyde (OPA) and fluorescence detection. From the results obtained it may be concluded that the most abundant free amino acids were Glu, Arg, Ala Asp, and Lys. None of the wine samples analysed had histamine (HIM) or Tyramine (TYM) levels above the limits considered as a possible toxic risk for healthy individuals. No measurable amounts of cadaverine (CAD) or methylamine (MEA) were found, showing no spoilage symptoms of sensory properties of the wines. Tryptamine (TRM) content was significantly higher in aged wines compared to young wines. However ethanolamine (ETA) content was lower. These data were used to make a preliminary classification of the samples using cluster analysis.     

保加利亚乳杆菌关键糖代谢机制的研究

以五株德氏乳杆菌保加利亚亚种为出发菌株,通过高效液相色谱法对四株后酸化强弱不同的保加利亚乳杆菌发酵的酸奶中葡萄糖、乳糖、半乳糖及乳酸的含量进行测定,通过Carrez法处理沉淀蛋白,采用AminexHPX87H色谱柱,5mmol/LH2SO4溶液为流动相,流速0.6mL/min。结果表明,本实验中保加利亚乳杆菌室温贮存过程中产乳酸的途径为乳糖到葡萄糖,葡萄糖通过糖酵解生成乳酸,生成的半乳糖不被利用,一直处于累积状态;后酸化强的菌株代谢乳糖和葡萄糖的含量比后酸化弱的菌株代谢量更高,乳糖代谢途径为菌株贮存期产酸关键途径。     

新疆熏马肠中生物胺含量的调查

利用高效液相色谱丹磺酰氯柱前衍生法,检测了从新疆自治区4个县市采集的44个熏马肠中8种生物胺含量。结果显示:4.6%熏马肠样品的生物胺(BAs)总量超过FDA规定的1 000 mg/kg限量标准,色胺、酪胺和亚精胺含量在不同程度上超过生物胺安全用量标准,腐胺和尸胺含量与国外报道基本一致。     

Isolation and structure elucidation of phenolic compounds from Cyclopia subternata Vogel (honeybush) intact plant and in vitro cultures

In the presented work, an insight was made into the polyphenolic composition of intact plant material and in vitro cultures of indigenous South African plant Cyclopia subternata Vogel (honeybush). Ethyl acetate fractions of methanol extracts were separated by means of gravity column chromatography and/or semipreparative HPLC on two serially connected monolithic RP-18 columns. The structures of the isolated compounds were determined by means of 1D and 2D NMR techniques and additionally confirmed by LC-DAD-ESI-MS. Apart from the previously described honeybush components, that is mangiferin (1), scolymoside (2), hesperidin (3) and narirutin (4), three additional compounds: iriflophenone 3-C-β-glucoside (benzophenone) (5), phloretin 3′,5′-di-C-β-glucoside (dihydrochalcone) (6), and isorhoifolin (flavone) (7) were identified for the first time in the herb of C. subternata. Additionally, three isoflavone glucosides, namely calycosin 7-O-β-glucoside (8), rothindin (9) and ononin (10), which had not been previously reported in Cyclopia plants, were identified in the callus of the above species. As far as the authors are concerned, this is the first report on the presence of benzophenone and dihydrochalcone derivatives in Cyclopia genus.     

Multi-residue method for determination of seven neonicotinoid insecticides in grains using dispersive solid-phase extraction and dispersive liquid–liquid micro-extraction by high performance liquid chromatography

A method using dispersive solid-phase extraction and dispersive liquid–liquid micro-extraction cleanup followed by high performance liquid chromatography (HPLC) has been established for determination of seven neonicotinoid insecticides residues in grains including brown rice, maize, millet and oat. Based on an appraisal of the characteristics of HPLC, validation experiments were conducted for seven neonicotinoid insecticides. In the method, dispersive solid-phase extraction was carried out using PSA and bonded C₁₈ coupled with graphitised carbon black with acetonitrile as the eluted solvent. In the linear range of each pesticide, the correlation coefficient was R² ? 0.99. At the low, medium and high three fortification levels of 0.05–0.8 mg kg⁻¹, recoveries fell within 76–123%. The relative standard deviation was between 0.9% and 12.6% for seven neonicotinoid pesticides. Low limits of detection (0.002–0.005 mg kg⁻¹) and quantification (0.007–0.018 mg kg⁻¹) were readily achieved with this method for all tested pesticides.     

A novel method for determining vitamin B1 in a wide variety of foodstuffs with or without polyphenols

Certain foodstuffs exhibit matrix interference effects on the vitamin B₁ analysis prescribed in the official methods of the European Union, AOAC International, and Japan. In this study, we demonstrated that one of the problematic polyphenols in green tea or cocoa was tannin. For these matrices, thiamine was found to interact with tannin in the extraction step and was thus removed by filtration as a residue. To resolve the matrix interference, we proposed lowering the pH of the extraction solution by adding hydrochloric acid after the enzyme reaction. High precision (2–3% RSDr) and good recovery (98.3–103%) were obtained with reference materials using the proposed method. We also confirmed the equivalence of the obtained data from the proposed method and the Japanese official method for nutritional labeling. From these results, the method was found to be effective for vitamin B₁ analysis regardless of the presence of interference matrices.     

Analysis of Phenolic Composition of Noble Muscadine (Vitis rotundifolia) by HPLC‐MS and the Relationship to Its Antioxidant Capacity

Abstract: Phenolic compounds and anthocyanins in muscadines have attracted much attention due to their diverse biological activities. With bioassays of antioxidant activities in terms of total phenolic content (TPC), total anthocyanin content (TAC), total procyanidin content (TPA), oxygen radical absorbance capacity (ORAC), and ferric reducing antioxidant power (FRAP) of different parts of the Noble muscadine, the butanol (BuOH) extract of the muscadine skin showed the highest TPC (317.91 ± 1.83 mg GAE/100 g FW), which might be ascribed to its high TAC of 227.06 ± 1.29 mg/100 g fresh weight (FW). The ethyl acetate (EtOAc) extract of the muscadine seed contained the highest TPA (55.30 ± 0.63 mg CE/100 g FW). Correlation analyses demonstrated a significant linear relationship of TPC and TAC compared to their ORAC and FRAP values within the range of R² from 0.9283 to 0.9936, which suggested that phenolics and anthocyanins in the extracts contributed significantly to their antioxidant potential. Nineteen individual phenolics and 5 anthocyanins were identified by HPLC‐MS, which indicated different chemical profiles of anthocyanins and other phenolics in the muscadine extracts. Practical Application: The paper has provided rich information of bioactive phytochemical profiles in different solvent extracts and their correlation with the antioxidant activity in the muscadine that is a very special regional fruit in U.S. Its high content of phenolic compounds demonstrates that muscadine could be beneficial to human health.     

大麦和麦芽萃取物抗氧化力的比较——采用高效液相色谱-库仑阵列检测器测定其游离酚类化合物含量

分析了10种大麦及其麦芽的热水浸出物的抗氧化能力.三价铁还原抗氧化能力(FRAP)和自由基消除能力(ABST)的值分别为,麦芽0.23～0.45mg GAE/gdw,大麦0.12～0.25mg GAE/gdw.无壳麦芽KM1910的抗氧化能力最强,而抗氧化力最高的大麦品种是Merlin.FRAP,ABST和ITT值之间存在着明显的正相关性(p<0.01).研究了施肥(20公斤N/公顷)对大麦抗氧化力的影响,结果表明施肥的影响并不明显,而基因类型对大麦抗氧化力影响明显.使用Folin-Ciocalteu's的方法测定总多酚含量,其范围在0.6～2.9mg GAE/gdw,与所有使用的测定抗氧化力的方法之间存在正相关性(p<0.01).采用配库仑阵列检测器的HPLC方法测定游离酚,含量最多的是阿魏酸,其含量范围是,大麦12.5～21.9μg GAE/gdw,麦芽7.8～56.μg GAE/gdw,大麦及麦芽中儿荼酸的含量范围分别为11.0～17.0μg GAE/gdw,0.9～12.1μg GAE/gdw.