HPLC法测定苹果浓缩汁中的多酚类物质

利用高效液相色谱法(HPLC)分析了儿茶素、绿原酸、咖啡酸、表儿茶素、香豆酸、阿魏酸等六种酚类物质在鲁加1号和鲁加5号苹果浓缩汁中的的含量.色谱条件:色谱柱为EdipseXDB-C18色谱柱(150mm×4.6mm id,5μm),以甲醇-1%乙酸水溶液作为流动相进行梯度洗脱.柱温30℃,流速为1.0ml/min,检测波长为280nm.在此色谱条件下,各组分均得到很好的分离.经测定鲁加1号苹果浓缩汁中含有儿茶素、绿原酸、咖啡酸、表儿茶素、香豆酸、阿魏酸等六种酚类物质;鲁加5号苹果浓缩汁中含有较少的绿原酸、咖啡酸、表儿茶素、香豆酸、阿魏酸等五种酚类物质.     

固相萃取-高效液相色谱法同时测定葡萄酒中没食子酸等8种多酚类化合物

建立了固相萃取.高效液相色谱光电二极管阵列检测法测定葡萄酒中没食子酸等8种多酚类生物活性化合物的方法.并用此方法测定了市售的7种葡萄酒中该8种生物活性物质的含量.实验确定了葡萄酒样品中的没食子酸等物质的固相萃取方法,通过优化萃取条件,有效的去除了葡萄酒中大量干扰成分.采用HypersilC18柱(250mm×4.6mm,i.d.5μm)分离.以乙腈-0.3%乙酸为流动相,线性梯度洗脱,以保留时间和特征光谱对分离出的组分予以定性确证,用峰面积进行定量.8种组分的质量浓度与其峰面积在一定的范围内有良好的线性关系,相关系数为0.9982～0.9999,8种组分的平均回收率为83.9%～103.7%(相对标准偏差为1.6%～4.6%),检测限为0.2～1.5mg/L.对市售的7种葡萄酒的检测结果表明,多酚类物质作为葡萄酒中重要的生物活性成分,其含量与葡萄酒的酿造方式,葡萄品种,葡萄产地有密切的关系.该方法简便、快速、灵敏,也适用于其它复杂体系中没食子酸等8种生物活性的成分分析.     

山楂多酚含量的反相高效液相色谱法测定

建立同时测定山楂中绿原酸、表儿茶素和芦丁3 种酚类物质的反相高效液相色谱方法,并研究这三种酚类物质在山楂干果果肉、干果果核和鲜果果肉中的含量。经测定,表儿茶素在山楂鲜果果肉中含量最高,达到(1.661 ± 0.024) mg/g;绿原酸和芦丁在山楂干果果肉中含量最高,分别达到(0.550 ± 0.002) mg/g 和(0.498 ± 0.002) mg/g。本方法样品处理简单,具有良好的重现性和线性,相关性系数均达到0.999,绿原酸、表儿茶素和芦丁的回收率分别为91.8%～110.9%、94.6%～107.9% 和94.2%～108.8%;检出限分别为0.14、0.37 和0.68μg/ml (S/N ＝ 3)。     

不同品种甜荞芽中酚类成分的比较

本文建立了甜荞芽5种酚类成分的测定方法,并且对7种甜荞芽中酚类成分进行比较分析。采用超高效液相色谱(UPLC)法检测甜荞中5种多酚成分含量,色谱条件为ACQUITYUPLC® BEHC₁₈色谱柱(2.1 mm×50 mm,1.7 μm),流动相甲醇(A)-0.20%冰乙酸水溶液(B),检测波长为254 nm,流速为0.20 mL/min,进样量为1 μL;并采用高效液相色谱法对甜荞芽中的矢车菊素-3-O-葡萄糖苷和矢车菊素-3-O-芸香糖苷成分的含量进行检测,用DPS 14.50软件对甜荞芽第7、10 d酚类成分的含量进行分析。结果表明,建立的超高效液相色谱法准确可靠,甜荞芽第7、10 d酚类成分总含量具有显著性差异(P<0.05),其中第7、10 d荭草素、异荭草素、牡荆素、异牡荆素、芦丁总含量最高的品种分别是赤甜1号、品甜2号,分别为43.66、40.82 mg/g,含量最低的品种分别是宁荞1号、定甜3号,分别为20.45、14.13 mg/g;矢车菊素-3-O-葡萄糖苷和矢车菊素-3-O-芸香糖苷总含量最高的分别是红花甜荞、宁甜1号,分别为218.47、282.95 mg/kg,最低的分别是赤甜1号、丰甜1号,分别为49.91、88.35 mg/kg。本实验为甜荞芽质量评价提供了依据,为后续研究奠定了基础。     

反相高效液相色谱法同时测定马铃薯块茎中酚酸类物质

目的：运用反相高效液相色谱法同时测定马铃薯中的绿原酸、咖啡酸、对香豆酸和阿魏酸。方法：色谱柱为YMC-C18(250mm×4.6mm,5μm),流动相为甲醇-水-冰醋酸(30:70:1,V/V)等度洗脱,柱温25℃,检测波长327nm。结果：绿原酸、咖啡酸、对香豆酸和阿魏酸在进样质量浓度分别为7.80～1000、0.78～100、0.312～40、0.078～10μg/mL范围内线性关系良好(r值范围0.9968～0.9999),平均回收率为92.38%～101.73%。结论：本法分析快速准确、灵敏度高、重现性好,江西、北京和新疆3个地域的环境条件对马铃薯的酚酸含量有一定的影响。     

果汁中9种酚酸类化合物的RP-HPLC-PAD分析

研究了同时测定5种果汁中没食子酸、儿茶酸、绿原酸、原儿茶酸、咖啡酸、表儿茶酸、阿魏酸、莽草酸和丁香酸等9种生物活性酚酸的反相高效液相色谱-光电二极管阵列检测新方法。采用ZorbaxEclipseXDB-C18色谱柱(5μm,250mm×4.6mmi.d.),流动相为甲醇-0.5%乙酸,梯度洗脱,流速1.0mL/min,以保留时间和特征光谱对分离出的组分予以定性确证,用峰面积进行定量。9种组分的质量浓度与其峰面积在一定的范围内有良好的线性关系,相关系数为0.9987～0.9999。9种组分的平均回收率为86.5%～98.8%(相对标准偏差为3.1%～5.8%)。检测限为0.2～1.0mg/L。结果表明,该方法也适用于其他复杂体系中没食子酸等9种生物活性成分的分析。     

Simultaneous Enantiomeric Determination of Acidic Herbicides in Apple Juice Samples by Liquid Chromatography on a Teicoplanin Chiral Stationary Phase

A novel and chiral liquid chromatography-ultraviolet method has been developed for simultaneous determination of mecoprop, fenoprop and diclofop acid herbicides. Optimization of mobile phase composition for enantiomeric separation on a teicoplanin stationary phase was done by experimental design and response surface analyses. When chiral separation of herbicide mixtures was optimized, multiple response analysis was necessary to determine combination of experimental factors, methanol percentage and triethylamine concentration in the aqueous buffer, which simultaneously optimize experimental responses. Under optimum conditions, acceptable resolution between the three enantiomeric pairs and between enantiomers of each studied herbicide was achieve in low analysis time. Applicability of the chromatographic method for simultaneous chiral herbicide determination was evaluated in commercial apple juice samples. Previously, a clean-up and preconcentration step on a polymeric solid phase extraction (SPE) cartridge (OASIS® MCX) was done. In order to get enantioresolution in the complex matrix, compatibility between the sample preparation procedure and the chiral liquid chromatography analysis was necessary. Thus, a focusing step was required after herbicide elution from the SPE sorbent to obtain an injection solution with low organic solvent composition. Detection limits were around maximum residue levels permitted by European Regulations in fresh fruit, allowing herbicide determination at enantiomer spiked levels from 0.075 to 0.750 μg g^?1, with recoveries in the range 65–99 % and relative standard deviations of ≤4 %. Due to co-extracted endogenous matter, which partially overlapped with mecoprop enantiomers, mathematical deconvolution was the best choice as integration tool minimizing errors in peak area estimation.     

固相萃取-高效液相法测定黄酒中多酚

为了寻找一种更高效、富集能力更强,更具有针对性的前处理方式,解决黄酒多酚测定时存在的杂质多、目标物含量低、定量不准确的问题,采用固相萃取小柱对黄酒进行前处理,就流动相条件、固相萃取小柱类型、洗脱剂类型、洗脱剂体积等因素对9种多酚的回收率影响做了评价比较,并运用该方法对不同甜型的绍兴黄酒中多酚质量浓度进行精确测定,结果表明:采用Poly-Sery HLB SPE小柱,甲醇为洗脱剂,洗脱体积为3倍上样体积时9种多酚回收率最高,均在87.3%～103.8%之间,相对标准偏差小于3.2%。不同甜型的绍兴黄酒中多酚以儿茶素和丁香酸为主,干型黄酒、半干型黄酒中多酚质量浓度低于甜型黄酒和半甜型黄酒。该方法具有快速、简便、准确的优点,可用于黄酒等酒类的多酚测定。     

Solid-Phase Extraction and Procedure for Determination of Phenolic Compounds in Maple Syrup

A solid phase extraction procedure was developed for the extraction of phenolic compounds from maple syrup. The list of targeted chemicals contains phenolic acids as well as aldehydes, flavanols and others such as coniferyl alcohol and 5-hydroxymethyl furfural. The procedure consists in passing a small quantity of maple syrup, 1 g diluted in 2 ml deionized water, through an Oasis HLB cartridge of 200 mg. The cleanest extracts were obtained by rinsing the cartridge load with formic acid 2 %/methanol (9:1). The analytes eluted with methanol were passed in an high-performance liquid chromatography (HPLC)-DAD system for analysis. The method performances show good recoveries; excluding gallic acid measured at 49 %, the chemical recoveries ranged from 81 to 119 %. Moreover, the method repeatability is less than 12 % (RSD) relative standard deviation for all chemicals except for epicatechin (20 %). The analysis method was applied for the determination of phenolic compounds in maple syrups from different color classes (Extra Light to Amber). Results show that concentrations of phenolic compounds vary among syrup classes and the greatest concentration was observed for the Amber syrups.     

高效液相色谱法测定菠萝中多酚类化合物

利用高效液相色谱法(HPLC)分析了多酚类物质在菠萝果皮、果肉、果心中的含量及分布情况。色谱条件：色谱柱为 Diamonsil C_(18)柱(250 mm×4．6 mm,5μm),流动相为乙腈和0．3%醋酸溶液,柱温为25℃,流速为 1．0mL/min,线性梯度洗脱,检测波长为280nm。在此色谱条件下,各组分均得到良好分离。经测定,菠萝果皮中含有4种酚类物质,为没食子酸、儿茶素、表儿茶素、阿魏酸,含量较高；果肉及果心中酚类物质为表儿茶素和阿魏酸,含量较低。     

Determination of 13 Phenolic Compounds in Rice Wine by High-Performance Liquid Chromatography

Rice wines are widely consumed by the general public in Asian countries, while comprehensive studies focused on the individual phenolic compounds in rice wines are limited. A rapid method for simultaneous determination of 13 phenolic compounds in rice wines by high-performance liquid chromatography (HPLC) was developed and validated, and the phenolic compounds in commercial rice wine samples (Chinese rice wine, Japanese sake, and Korean makgeolli) were determined in this paper. The identified compounds contained gallic acid (GA), protocatechuic acid (PRCA), vanillic acid (VA), syringic acid (SRA), caffeic acid (CA), ferulic acid (FA), p-coumaric acid (pCA), sinapic acid (SA), chlorogenic acid (CHA), (+)-catechin (CAT), (?)-epicatechin (EPI), quercetin (QUE), and rutin (RUT). Phenolics were separated with a C18 reversed-phase column at 38 °C by gradient elution using 3 % acetic acid aqueous solution (solvent A) and acetonitrile (solvent B) (0 min, 5 % B; 5 min, 8 % B; 10 min, 15 % B; 20 min, 25 % B; and 25 min, 5 % B) as the mobile phase at 280 nm with flow rate of 1.0 mL min^?1. With direct injection of rice wine samples, the chromatograms of all analytes were observed within 20 min, all calibration curves were linear (R ²?>?0.995) within the range, limits of detection (LOD) ranged from 0.02 to 0.06 μg mL^?1, and good recoveries (88.07–106.80 %) and precision (relative standard deviation (RSD)?<?5.36 % ) were obtained for all compounds. This method was applied to quantify phenolic compounds in commercial rice wine samples (Chinese rice wine, Japanese sake, and Korean makgeolli), and good separation peaks were observed and catechin was the predominant phenolic in the samples. The average values of total phenolic contents of the three groups of rice wine were significantly different (p?<?0.01). In conclusion, this procedure can be used to determine the phenolic compounds in various types of rice wines, as well as to characterize and differentiate rice wine samples.     

高效液相色谱法测定糜子中酚酸类化合物

为探索糜子麸皮和糜米中酚酸类物质的成分和含量,采用福林-酚法和高效液相色谱法测定比较糜子麸皮 和糜米中自由酚含量和酚酸类物质的种类。结果表明：不同品种糜子麸皮之间自由酚含量差异不显著,糜米之间自 由酚法差异极其显著（P＜0.01）。同一品种糜子麸皮和糜米之间自由酚含量差异显著（P＜0.05）,糜子麸皮自由 酚含量远高于糜米。赤糜2号麸皮和糜米中自由酚含量最高,麸皮中为159.22 mg没食子酸/100 g,糜米中为47.98 mg 没食子酸/100 g。糜子中检测到的酚酸类物质有绿原酸、丁香酸、香草酸、p-香豆酸、阿魏酸。     

高效液相色谱-四极杆飞行时间串联质谱法解析桑椹酒渣中的酚类物质

该研究通过研究桑椹酒渣中的酚类化合物,为开发酒渣的价值提供一定的理论基础和数据支撑。建立云桑二号桑椹酒渣中的酚类化合物的高效液相色谱-四极杆飞行时间串联质谱法（HPLC-Q-Time-of-Flight Mass Spectrometry,HPLC-Q-TOF-MS）定性分析方法。液相色谱使用ZORBAX SB-Aq(2.1 mm×100 mm,1.8-Micron）色谱柱,流动相为乙腈和0.1%(V/V）甲酸水溶液,梯度洗脱,采用ESI离子源在负离子模式进行质谱检测。最终鉴定出云桑二号桑椹酒渣中酚类物质共14种。然后利用标准品对照高效液相色谱法（High Performance Liquid Chromatography,HPLC）对高效液相色谱-四极杆飞行时间串联质谱法鉴定出的多酚类化合物进行了定量测定,发现桑椹酒渣中的酚类物质组成与桑椹大致相同。但各单体酚含量总体降低。其中,花青素类酚类物质含量最高的是天竺葵素-3-葡萄糖苷（718.30μg/g）,非花青素类多酚物质含量最高的是儿茶素（1 805.87μg/g）。这些结果表明桑椹酒渣酚类含量丰富,是开发健康食品的良好原料。     

微波处理对萌动亚麻籽酚类化合物油相迁移的影响

强化亚麻籽中主要酚类化合物内源性合成和油相迁移对提升亚麻籽油氧化稳定性,最大限度地增加α-亚麻酸生物利用率尤为重要。探究了适度萌动(25℃,24h)联合微波处理(700W,1~5min)对压榨亚麻籽油得率和色泽、脂质构型和结晶熔融性、抗氧化活性和氧化稳定性的影响,并研究了亚麻籽中木酚素和游离酚酸的释放及油相迁移规律。结果表明:单一萌动处理(24h)后亚麻籽油得率降低了7.39%(P<0.05),而进一步微波处理后油脂得率增加了29.31%(P<0.05),这主要归因于微波处理破坏了亚麻籽中油脂体膜结构完整性,导致膜内中性脂质外溢、融合和胞外渗透。微波处理1~5min过程中,亚麻籽油中以LnLnLn构型存在的C18∶3ω3质量分数呈现明显升高趋势,同时总磷脂质量摩尔浓度以及磷脂酰乙醇胺、磷脂酰甘油、磷脂酰肌醇占比显著增加(P<0.05),但未明显影响油脂的结晶行为和熔融特性。与未处理组相比,微波处理5min降低了初级和次级氧化产物水平,显著改善了亚麻籽油的氧化稳定性和抗氧化活性(P<0.05),这主要归因于木酚素大分子及其解聚产物开环异落叶松树脂酚二葡萄糖苷,以及游离酚酸香兰素、香草酸和阿魏酸的油相富集。研究阐释了萌动联合微波预处理对亚麻籽油品质特性的影响,旨在为亚麻籽油提质制取和亚麻籽高值化利用提供理论依据。     

高效毛细管区带电泳法同时检测3个产地沙棘果粉中的活性物质

利用高效毛细管区带电泳法,对3个产地沙棘果粉中的芦丁、山柰酚、异鼠李素、槲皮素4种活性物质进行同时分离测定。考察不同电泳条件对分离效率的影响,得出最佳电泳条件:缓冲溶液20 mmol/L Na_2B_4O_7-H_3BO_3(质量浓度为1.5 mg/mL的β-环糊精),pH 9.55,检测波长370 nm,分离电压25 kV,进样时间5 s。在该条件下,芦丁、山柰酚、异鼠李素、槲皮素4种活性物质在11 min内得到分离,线性范围分别为0.01~0.51、0.05~0.93、0.02~0.65、0.03~0.81 mg/mL,相关系数在0.997 1~0.999 1之间,检出限分别为5.05×10~(-5)、2.10×10~(-5)、3.75×10~(-5)、1.31×10~(-5) mg/mL(RSN=3),各物质线性关系良好。日内及日间精密度范围为0.08%~4.72%,平均回收率在95.51%~104.66%之间,相对标准偏差不大于3.92%(n=3)。在优化条件下,对4种活性物质标准品的混合物进行测定,并用相同方法对3个产地沙棘果粉中活性物质的提取液进行检测。结果表明:不同产地沙棘中,4种被检测化合物的含量各不相同。沙棘中被测4种化合物总量最高的产自新疆乌鲁木齐,最低的产自甘肃武威,而槲皮素含量以产自山西吕梁的最高,山柰酚和异鼠李素以产自新疆乌鲁木齐最高。本方法快速简便、准确可靠,可用于沙棘果粉中多种活性物质的同时检测。     

两种芦笋不同部位酚类物质及抗氧化活性研究

采用超声辅助法提取白芦笋茎、白芦笋尖、绿芦笋茎和绿芦笋尖中的酚类物质,通过比色法及高效液相色谱(high performance liquid chromatography,HPLC)法测定各提取物中总酚、总黄酮、总单宁、缩合单宁和芦丁含量及其抗氧化能力(DPPH自由基、ABTS自由基清除活性和还原力),并探究芦笋酚类物质与抗氧化能力之间的相关性。结果表明,两种芦笋中均不含单宁类物质;绿芦笋尖中总酚、总黄酮、芦丁含量最高,3种抗氧化活性均最强,其后依次为绿芦笋茎、白芦笋尖和白芦笋茎。HPLC指纹图谱显示,绿芦笋尖中酚类物质的种类及含量均最高,白芦笋茎中则最少。以上结果说明绿芦笋比白芦笋中酚类物质更多,抗氧化性更强,且芦笋尖中酚类含量及抗氧化性优于芦笋茎。相关性分析发现,芦笋中总酚、总黄酮、芦丁、DPPH自由基和ABTS自由基清除能力两两之间均显著正相关,表明芦笋中酚类物质与自由基清除能力关系密切。     

Comparison of Different Extraction Methods to Determine Phenolic Compounds in Virgin Olive Oil

A comparison between different extraction methods has been performed in order to assess their effectiveness for the analysis of total phenols (liquid–liquid extraction (LLE), liquid–liquid micro extraction (LLME), and ultrasound liquid–liquid extraction (USE)) and individual phenols (LLME, USE, and solid-phase extraction (SPE)) from virgin olive oil (VOO). Statistical analysis of the analytical data obtained for the total phenol content of a VOO, showed that LLME and USE can represent a reliable alternative to the traditional procedure based on LLE that needs more amount of sample, generates more wastes, and is more time consuming. When an olive oil spiked with phenols was used to test the efficiency of LLME, USE, and SPE methods, the statistical analysis of the data obtained for each individual phenol, again proved LLME and USE methods to be the most suitable, in terms of precision and recoveries, for this purpose. The analysis of real samples (Arbequina and Picual cultivars) confirmed the results obtained for the spiked oil.     

猴头菇醇提物及其不同极性部位酚类物质定量分析

利用超高效液相色谱-电喷雾质谱(ultra performance liquid chromatography-electro spray ionization-mass spec-trometry,UPLC-ESI-MS)对猴头菇醇提物(ethanol extract,EE)及其石油醚萃取物(petroleum et...     

RP-HPLC-DAD法测定茶叶籽油酚类化合物

建立同时分离、检测茶叶籽油中酚类化合物组分和含量的高效液相色谱法。比较了流动相组成的影响,选择合适的乙酸加入量,建立最优梯度洗脱条件。结果表明,14种酚类物质在该条件下能够得到较好的分离,各物质的线性相关系数均在0.99以上。运用该方法从茶叶籽油中共检测到13种酚类化合物,包括5种酚酸、3种黄酮类和5种儿茶素类,含量分别为46.8、21.72、40.16μg/g;其酚酸类主要为肉桂酸和咖啡酸,黄酮类主要为山奈酚、槲皮素和芦丁,儿茶素类主要为儿茶素。该方法准确、可靠,适用于茶叶籽油中酚类化合物分析。