番茄及其制品中番茄红素含量的C18-HPLC-PDA定量分析

目的:建立一种可靠的测定番茄及其制品中番茄红素含量的C18-HPLC-PDA方法。色谱条件:固定相为DIAMONSILTM柱(Dikma Technologies,250×4.6mm,5μm);流动相A为乙腈:水(9:1);流动相B为乙酸乙酯;线性梯度洗脱:在15min内,流动相B由0%增为100%(V/V),随后5min,流动相B保持100%;流速1.0ml/min,PDA波长范围260～600nm;色谱图检测波长471nm;进样量20μl;柱温=室温。结果:此方法的定量限为0.10μg/ml,质量浓度在0.10～25.60μg/ml范围内浓度与组分峰面积的线性相关系数为0.9994,RSD为2.6%,回收率为99.3%。结论:这是一种番茄及其制品中番茄红素含量测定的可靠方法。     

超声波辅助-HPLC测定芝麻油中木脂素含量

以超临界CO2流体萃取的芝麻油为原料,采用超声波辅助甲醇萃取法对芝麻油进行前处理,并通过高效液相色谱法测定芝麻油中木脂素含量。结果表明,芝麻素和芝麻林素色谱峰分离效果好,干扰峰少,芝麻素与芝麻林素平均加标回收率分别为99.3%、96.2%,相对标准偏差分别为0.87%、1.71%。与皂化法前处理方法相比,此方法的前处理简便快速、结果准确、灵敏度高、稳定性好,适用于芝麻油中芝麻素和芝麻林素含量的测定。     

HPLC法测定芝麻油中芝麻素的含量

研究了以芝麻油为原料,采用氧化铝层析柱预处理得到芝麻素混合物,再用高效液相法进行含量的检测.色谱条件:色谱柱:Inertsil(ODS-3 250 mm×4.6 mm,5μm);流动相:甲醇:水=70:30(V/V);流速:2 mL/min;检测器:惠普1050紫外检测器;柱温:30℃.测定结果表明,被测峰与其他峰可完全分离,线性范围5～200μg/mL,相关系数r=0.9999,平均回收率100.6%.方法简便、准确、灵敏度高,可用于芝麻素含量的测定.     

正相高效液相色谱法同时测定芝麻油中生育酚、芝麻素及芝麻林素含量

建立了正相高效液相色谱法同时测定芝麻油中生育酚(α-、β-、γ-、δ-生育酚)、芝麻素及芝麻林素含量的方法。样品经正庚烷溶解后,在二醇基硅胶色谱柱上以四氢呋喃-正庚烷溶液洗脱、荧光检测器分析。结果表明:芝麻素及芝麻林素荧光特性良好,样品分析在20 min内完成;方法学评价结果显示生育酚在1.0~5.0μg/m L、芝麻素及芝麻林素在0.1~5.0μg/m L范围内线性关系良好,相关系数R~2均大于0.99;生育酚、芝麻素以及芝麻林素的检出限为0.29~0.74 mg/kg,定量限为0.91~2.10 mg/kg;6种化合物加标回收率为83.47%~104.57%,相对标准偏差为0.38%~6.55%。采用该方法分析了12个芝麻香油、冷榨芝麻油、浸出成品芝麻油中生育酚、芝麻素以及芝麻林素含量,发现芝麻油中生育酚以γ型为主,芝麻素、芝麻林素含量较高。该方法简单、灵敏度高、重复性好,可用于芝麻油中生育酚、芝麻素及芝麻林素含量的同时检测。     

不同产地和品种芝麻营养成分差异分析

为分析不同产地和品种芝麻之间营养品质差异，以及营养品质之间的相关性，选取了山东省、河北省和湖南省200份芝麻样品，测定芝麻中脂肪、蛋白质、芝麻素和芝麻林素含量，并进行差异性和相关性分析。结果表明，不同芝麻品种之间蛋白质、脂肪、芝麻素和芝麻林素的平均含量分别为27.07%、52.27%、3.34 g/kg和1.48 g/kg。不同种皮颜色的芝麻营养品质略有差异，但差异不显著。山东省和河北省芝麻的蛋白质、脂肪含量显著高于湖南省芝麻(P<0.05)。河北省芝麻的芝麻素含量显著高于湖南省(P<0.05)，但山东省、湖南省之间差异不显著。3个省份之间的芝麻林素含量差异不显著。蛋白质与脂肪含量间呈极显著负相关(P<0.01)，芝麻素与脂肪含量间呈显著正相关，相关系数为0.145(P<0.05)，这与之前的研究结果一致。芝麻素与芝麻林素含量间呈极显著正相关(P<0.01)。蛋白质、脂肪与芝麻林素之间相关性不显著。     

HPLC法测定不同品种苹果中原花青素B2的含量

目的：建立苹果中原花青素B2含量的测定方法,测定5个不同品种苹果果皮和果肉中原花青素B2的含量。方法：采用HPLC法测定苹果果皮和果肉中原花青素B2的含量,色谱柱为Phenomenex Luna C18柱 (250mm×4.6mm,5μm);流动相：A相：0.5%磷酸溶液,B相：水-乙腈(50:50,V/V);流速：1.0mL/min;柱温：30℃;检测波长：280nm。结果：原花青素B2进样量在2.399～9.596μg范围内与峰面积线性关系良好(R2＝0.9998),回收率97.72%,RSD=1.98%。经测定几种苹果果皮和果肉中原花青素B2的含量分别在275.24～548.42μg/g和90.19～247.06μg/g范围中。结论：本法简便、易行,可用于苹果质量控制。     

高效液相色谱法测定玉米须中刺芒柄花素的含量

目的：建立玉米须中刺芒柄花素含量测定的方法。方法：运用高效液相色谱法测定,色谱柱为HypersilC18 (4.6mm × 250mm,5μm),流动相为甲醇-0.1% 磷酸(55:45,V/V),流速0.8ml/min;检测波长254nm。结果：刺芒柄花素在2.3～23μg/ml 范围内线性关系良好,r=0.9991。平均回收率为96.93%,RSD 为1.30%。结论：本法方便、准确,可以用于玉米须的质量控制。     

高效液相色谱法测定芝麻油中芝麻素及芝麻林素

建立高效液相色谱(HPLC)法测定芝麻油中芝麻素和芝麻林素的方法。结果表明：方法以甲醇-水为流动相，梯度洗脱；提取溶剂为乙腈；净化剂为50 mg硅胶键合乙二胺-N-丙基(PSA)+50 mg C₁₈;芝麻素和芝麻林素在1～100μg/mL范围内呈线性关系，相关系数(r)均大于0.998;方法检出限(LOD)为0.03 mg/g、定量限(LOQ)为0.06 mg/g。加标回收率和相对标准偏差(RSD)均符合GB/T 27417—2017的要求。方法前处理操作简单、重复性好，适用于芝麻油中芝麻素和芝麻林素的测定。     

芝麻油中芝麻素、芝麻林素和细辛素检测方法优化

采用有机溶剂甲醇提取、HPLC同时分析芝麻油中芝麻素、芝麻林素和细辛素含量。为提高分析质量与准确性,优化甲醇提取溶剂用量和超声辅助提取的时间,并对检测方法进行方法学考察。结果表明：最佳提取条件为甲醇用量10 mL（芝麻油0.1 g）,超声时间2 min;芝麻素、芝麻林素和细辛素线性范围分别为4～100 mg/L、4～100 mg/L和1～40 mg/L,线性关系良好,相关系数分别为0999 5、0.999 6和0.999 2;芝麻素、芝麻林素和细辛素的检出限分别为0.03、0.02 mg/g和0.02 mg/g,定量限分别为0.06、0.06 mg/g和0.04 mg/g,加标回收率分别为87.17%～92.59%、9271%～102.24%和95.66%～108.93%,加标回收率的相对标准偏差均小于5%,方法的稳定性、准确性和精密度均符合检测要求。该方法操作简单、耗时短(完成一次分析只需30 min)、成本低、稳定性高,能有效应用于芝麻油中3种木脂素组分的分析检测。     

HPLC法测定龙眼肉中的几种核苷类物质

目的:建立HPLC法测定龙眼肉中腺苷、尿苷和腺嘌呤的含量。方法:采用NucleosilC18反相柱(250mm×4mm),以0.01mol/L的KH2PO4:乙腈=92:8为流动相,流速为1ml/min,检测波长为254nm,柱温40℃,用外标法,测定了龙眼肉中腺苷、尿苷和腺嘌呤的含量。结果与结论:分析中选取腺苷的线性范围0.1～20.0μg/ml,相关系数r=0.9999,回收率94.59%,RSD3.10%;尿苷的线性范围0.05～10.0μg/ml,相关系数r=1,回收率97.49%,RSD4.50%;腺嘌呤线性范围0.05～10.0μg/ml,相关系数r=1,回收率103.11%,RSD1.90%。该方法简便快速,线性关系良好。     

Variation of sesamin,sesamolin and tocopherols in sesame (Sesamum indicum L.) seeds and oil products in Thailand

Sesame (Sesamum indicum L.) seed and oil contain abundant lignans, including sesamin, sesamolin and lignan glycosides. The aim of the present study was to determine sesamin, sesamolin and tocopherol contents in sesame seed and oil available in Thailand. The results showed that there was a large variation of sesamin and sesamolin contents in products. The distribution plot of sesamin and sesamolin contents in seeds showed that the mean values of sesamin and sesamolin were 1.55 mg/g (SD = 1.63; range n.d.–7.23 mg/g) and 0.62 mg/g (SD = 0.48; range n.d.–2.25 mg/g), respectively. The range of total tocopherols of these sesame lines was 50.9–211 μg/g seed. In commercial sesame oils, the ranges of sesamin and sesamolin were 0.93–2.89 mg/g oil and 0.30–0.74 mg/g oil, respectively, and tocopherol contents were 304–647 μg/g oil. The study reveals the extensive variability in sesamin, sesamolin and tocopherol contents among sesame products.     

芝麻核心种质芝麻素和芝麻酚林的关联分析

选用来源我国黄河流域至长江流域8省215份芝麻核心种质材料,对其种子中芝麻素（sesamin）和芝麻酚林（sesamolin）含量进行测定,芝麻素平均值5．24mg／g,变异范围为0．88～11．05mg／g,变异系数38．56％,芝麻酚林平均值3．30mg／g,变异范围为0．93—6．96mg／g,变异系数22．68％,二者均符合正态分布,且相关分析表明两者间呈极显著正相关;采用标记一性状关联分析法,进行芝麻素和芝麻酚林与SSR、SRAP、AFLP标记的关联分析。利用GLM模型共检测到33个标记与芝麻素和芝麻酚林极显著（P〈0．01）关联,同时与两种成分显著关联的有4个;利用MLM模型共检测到8个显著关联的标记,与两种成分显著关联的分别有4个;其中SSR标记SSll82-3在两种模型中同时极显著关联到芝麻素和芝麻酚林,且解释率较高。该研究将为芝麻功能性成分遗传改良和分子标记研究奠定重要基础。     

不同品种类型芝麻品质性状的比较分析

为全面分析不同品种类型芝麻的品质性状及其与重要农艺性状间的关系,筛选294个代表性芝麻品种资源,通过多点种植和测定籽粒脂肪、蛋白质、芝麻素和芝麻林素含量,对不同品种类型芝麻的品质性状进行了差异比较,并对品质性状之间和品质性状与农艺性状的相关性进行了分析。结果表明,294个芝麻品种脂肪、蛋白质、芝麻素和芝麻林素平均含量分别为52.77%、20.41%、310 mg/g和1.92 mg/g。不同株型芝麻,单秆型品种脂肪、芝麻素含量极显著高于分枝型品种,蛋白质含量显著低于分枝型品种,芝麻林素含量差异不显著;不同叶腋花数芝麻,单花型品种脂肪、芝麻素含量极显著低于三花型品种,蛋白质含量极显著高于三花型品种,芝麻林素含量显著低于三花型品种。不同品种芝麻脂肪含量与蛋白质含量呈极显著负相关,与芝麻素、芝麻林素含量呈极显著正相关;蛋白质含量与芝麻素、芝麻林素含量呈极显著负相关;芝麻素与芝麻林素含量呈极显著正相关;脂肪含量与生育期、籽粒颜色L*值、b*值呈极显著正相关,与千粒重、籽粒长度、宽度、长宽比和籽粒颜色a*值呈极显著负相关;蛋白质含量与千粒重、籽粒长度、籽粒宽度、籽粒长宽比呈极显著正相关,与生育期、籽粒颜色L*值及b*值呈极显著负相关,与籽粒颜色a*值相关性不显著;芝麻素含量与生育期呈显著正相关,与籽粒长宽比、籽粒颜色L*值及b*值呈极显著正相关,与千粒重、籽粒长度呈极显著负相关,与籽粒宽度、颜色a*值相关性不显著;芝麻林素含量与生育期、籽粒颜色a*值及b*值呈极显著正相关,与千粒重、籽粒长度、籽粒宽度呈极显著负相关,与籽粒长宽比、籽粒颜色L*值相关性不显著。     

Extraction,separation and characterisation of sesame oil lignan for nutraceutical applications

Nutraceutical aspects of sesame oil (SO) are well reported. However, an efficient process for commercial production has not yet been reported. In this study we have aimed at separating lignans from SO aiming at use as nutraceuticals. SO was subjected to sequential extraction with methanol under selected conditions of temperature (70 °C), time (100 min) and solvent:oil ratio (1:1). Under the optimised conditions, the yields of pooled methanolic extract concentrate and residual oil were 10.09 ± 1.0 g and 89.2 ± 1.0 g, respectively. On HPLC analysis, the methanol concentrate showed a total lignan content of 9.32 ± 0.19% (6.54 ± 0.12% sesamin and 2.78 ± 0.31% sesamolin). The concentrate was subjected to low temperature crystallization (4 °C) for the separation of lignan crystals and 51% of the lignans in the oil with 94.4% purity. The crystal-removed methanolic concentrate was saponified and purified; the total lignan content (sesamin and sesamolin) in the unsaponifiable matter (USM) was 64%.The distribution of sesamin and sesamolin in the purified USM was in the proportion 46:54, unlike that in the pure crystals (84:16). Lipid classes (triglycerides, TG; free fatty acids, FFA; diglycerides, DG; monoglycerides, MG; polar lipid, PL) in SO, methanolic extract concentrate and residual oil were separated using thin-layer chromatography (TLC). The amounts of lipid classes were determined by relating the total area of the fatty acid peaks to the area of the peak for internal standard (methyl heptadecanoate), using gas chromatography (GC). The process reported here describes a simple and less cumbersome procedure to produce lignans with high yield and purity for nutraceutical applications.     

Effect of refining on the lignan content and oxidative stability of oil pressed from roasted sesame seed

Oxidative stability of pressed and refined sesame oils during seven consecutive months of storage at room temperature was studied comparatively. Lignans, peroxide value (PV), p‐anisidine value (AV) and total oxidation value (TOTOX) were determined as evaluation indices. PV, AV and TOTOX of sunflower, corn and peanut oils were simultaneously monitored to compare their oxidative storage stabilities with the sesame oils. The total amount of lignans in the pressed and refined sesame oils were 1103 and 790 mg per 100 g respectively. The contents of sesamin and sesemolin in the pressed sesame oil were 734 and 369 mg per 100 g respectively. Sesamin and sesamolin content were reduced by 256 and 159 mg per 100 g, respectively, after refining. Nearly 40% of the sesamin epimerised to asarinin after oil refining. The results indicate that sesame oils pressed from roasted seed have far superior storage stability to oxidation than the other vegetable oils. This difference may be due to much higher sesamin and sesamolin contents in the pressed sesame oils. The results suggest lignan compositions and levels could be used as key indicators for evaluating the oxidative storage stability of sesame oil products as well as to differentiate between pressed and refined sesame oils.     

高效液相色谱-光电二极管阵列检测器法测定野山楂中两组分的含量

【摘要】 建立高效液相色谱法测定了野山楂中乌索酸和齐墩果酸的含量,同时采用光电二极管阵列检测器检测两组分的紫外光谱。色谱柱为NucleosilC18柱(4.6mm×250mm,5μm),流动相为甲醇-水(87:13,V/V),流速0.8ml/min,检测波长210nm,柱温26℃。乌索酸在0.1244～2.488μg范围内线性关系良好(r=0.9996),平均回收率为98.1%。齐墩果酸在0.1192～2.384μg范围内线性关系良好(r=0.9999),平均回收率为101.2%。方法简便、准确、重现性好、线性范围宽,适用于测定野山楂中乌索酸和齐墩果酸的含量。     

单扫描示波极谱法连续测定榛蘑中的锌、铁、锰

本文对单扫描示波极谱法同时测定榛蘑中的锌、铁、锰微量元素的含量进行了研究,选用0.4mol/L乙二胺-2.5×10-3mol/L三乙醇胺-0.1mol/L硫氰酸钾为底液。锌、铁、锰峰电位分别为-1.46V、-1.69V、-1.78V(υs.SCE),线性范围:0.2～1.2μg/ml Zn、0.2～1.6μg/ml Fe、0.04～0.5μg/ml Mn,锌、铁、锰的检出限分别为0.015μg/ml、0.024μg/ml、0.018μg/ml,回收率为96.6%～103.3%。此方法准确、简便、快速、灵敏度高。     

Microwave Heating Affects Composition and Oxidative Stability of Sesame (Sesamum indicum) Oil

The effects of microwave heating on antioxidative components and lipid quality of sesame seeds were studied. Amounts of antioxidative components were 576, 18, and 8 mg/kg oil for γ-, δ-, and α-tocopherols; 6,824, 5,642, and 54 mg/kg oil for sesamin, sesamolin, and sesamol, respectively. During microwave treatments, concentrations of tocopherols, sesamin and sesamolin gradually decreased, and ca. 20% of these dominant components was lost after 30 min heating. However, microwave treatments for 16 to 20 min, which would be optimal to prepare sesame oil with better quality, still retained over 85% of the antioxidative components (with few exceptions) and caused no significant chemical changes in lipids.