芝麻油生产工艺对细辛素形成的影响研究

通过对不同制油工艺制得的28个芝麻油样中芝麻木酚素组分含量(尤其是细辛素含量)进行的检测分析,研究制油工艺对芝麻油中细辛素含量的影响。结果发现：2个浸出精炼芝麻油样中细辛素含量平均119.45 mg/100g,其他26个油样中仅有3个检测出少量细辛素,分别为17.25 mg/100g、7.43 mg/100g、0.58 mg/100g,冷榨芝麻油中未检出细辛素。对不含细辛素的冷榨芝麻油进行水化脱胶、碱炼脱酸、吸附脱色、蒸馏脱臭等精炼处理,并对处理后的芝麻油进行细辛素含量检测分析。结果表明：添加磷酸进行水化脱胶和添加活性白土进行吸附脱色能造成芝麻油中细辛素的形成,且随脱胶时磷酸添加量和脱色时白土添加量的增加,细辛素含量增加(磷酸添加量1%时为131.22 mg/100g,白土添加量5%时为50.73 mg/100g);碱炼脱酸、活性炭脱色、水蒸汽蒸馏脱臭过程只降低了芝麻木酚素总量,没有细辛素形成。据此,细辛素可作为区别冷榨芝麻油和其他芝麻油尤其是浸出精炼芝麻油的特征指标。     

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。     

芝麻油生产工艺对细辛素形成的影响

对28个芝麻油样的芝麻木酚素组分含量进行检测分析。结果发现:2个浸出精炼芝麻油样中细辛素含量(mg/100 g)平均119.45,其他26个油样中仅有3个检测出很少的细辛素(分别为17.25、7.43、0.58),冷榨芝麻油中未检出细辛素。对冷榨芝麻油进行水化脱胶、碱炼脱酸、吸附脱色、蒸馏脱臭等精炼处理,并对处理后的芝麻油进行细辛素含量检测。结果表明:磷酸水化脱胶和活性白土吸附脱色能造成芝麻油中细辛素形成.且含量随磷酸用量和白土用量的增加而增加(磷酸用量1%时为131.22,白土用量5%时为50.73);其他处理过程没有细辛素形成。据此,细辛素可作为区别冷榨芝麻油和浸出精炼芝麻油的特征指标。     

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。     

芝麻素与细辛素检测方法及生物活性的研究进展

旨在为芝麻木酚素相关产品、特殊用途油脂等的研发提供参考,对芝麻木酚素中主要的脂溶性活性成分芝麻素及其转化产物细辛素的含量分布、转化条件、检测方法和生物活性进行综述。芝麻素是芝麻中含量最多的脂溶性木酚素,而芝麻中几乎不含细辛素,但芝麻素可在酸性和受热条件下转化为细辛素;芝麻素与细辛素的检测方法有高效液相色谱法、薄层色谱法、气相色谱-质谱联用法、液相色谱-质谱联用法等;芝麻素具有抑菌、抗癌、降血脂等生物活性,细辛素具有抗炎、抑菌、抗病毒、抗癌、抗肿瘤、抗氧化等生物活性。     

米酒乳杆菌素分离纯化条件研究

目的：对米酒乳杆菌产生的广谱细菌素进行分离纯化技术研究。方法和结果：采用活性炭脱色、冷乙醇沉淀、Sephadex G50 葡聚糖凝胶层析和高效液相色谱技术对米酒乳杆菌产生的细菌素进行分离纯化。结果表明,发酵浓缩液脱色的最佳工艺条件为活性炭加量3.5%、温度40℃、脱色时间20h,脱色率达64.5%。冷乙醇沉淀的最佳乙醇终浓度为80%,葡聚糖凝胶层析的洗脱液流速为0.5ml/min,上样量3ml,高效液相色谱纯化的流动相为90% 的甲醇水溶液,在此条件下可得到电泳纯的细菌素。结论：确定了米酒乳杆菌素的分离纯化条件,为细菌素的理化性质和抑菌机理的研究提供依据。     

高效液相色谱法同时测定芝麻制品中木脂素及生育酚含量的研究

建立了高效液相色谱法同时测定芝麻制品中3种木脂素及生育酚含量的研究方法。以市售芝麻油和黑、白芝麻酱为原料,优化了超声波前处理条件,样品经超声波辅助甲醇萃取后,利用Symmetry C18色谱分离柱,以甲醇-水为流动相进行梯度洗脱。结果表明:超声波前处理最佳条件为超声波功率320 W、料液比1∶120(芝麻油)、料液比1∶80(芝麻酱)、超声时间20 min; 3种木脂素和生育酚平均回收率在88. 5%～108. 4%之间,精密度在2. 4%～4. 8%之间,检出限为0. 43～0. 98mg/kg,定量限为1. 33～2. 84 mg/kg,木脂素及生育酚类化合物分离效果好。     

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。     

植物乳杆菌JLA-9产细菌素的分离纯化

将来源于东北传统发酵酸菜中的植物乳杆菌JLA-9产的细菌素进行分离纯化,首先利用饱和度为80%的硫酸铵溶液对发酵上清液进行沉淀粗分离。复溶后利用Sephadex LH-20进行凝胶层析纯化,之后采用Hitrap QFF进一步进行离子交换层析纯化,利用反相高效液相色谱(Reversed-Phase High Performance Liquid Chromatography,RP-HPLC)C_(18)柱进行最终纯化,得到单一活性抑菌组分,说明细菌素得到基本纯化,经基质辅助激光解吸电离飞行时间质谱(Matrix-Assisted Laser Desorption/Ionization Time of Flight Mass Spectrometry,MALDI-TOF/MS)确定该细菌素的分子质量约为0.9 kDa左右。采用琼脂扩散法测定了细菌素对常见的食源性致病菌和腐败菌的抑菌效果,结果显示该细菌素具有较好的抑制作用。     

大孔吸附树脂对高良姜素吸附纯化特性的研究

目的:研究大孔吸附树脂分离纯化高良姜中高良姜素的工艺条件及参数。方法:以高良姜素的吸附率和解吸率为考察指标,从中筛选树脂,并研究大孔吸附树脂分离纯化高良姜素的吸附性能和洗脱参数。结果:HPD-600树脂对高良姜素有较好的吸附分离性能,适合于从高良姜中提纯高良姜素,经该树脂吸附解吸,饱和吸附率为91.8%,解吸率85.36%。结论:大孔吸附树脂分离纯化高良姜素的纯度可达92.4%,而上柱前初提物中高良姜素纯度为59.4%,说明采用本方法分离纯化高良姜素是可行的。     

高效液相色谱法测定芝麻油中的苯并(a)芘含量

建立高效液相色谱法(HPLC)测定芝麻油中苯并(a)芘含量的方法.适量样品溶解于正己烷中,经中性氧化铝柱吸附,用正己烷洗脱苯并(a)芘,采用荧光检测器检测.苯并(a)芘在0.1～20 gL范围内呈线性关系,线性方程为y=21.226x-0.7335,R2=0.9998;对芝麻油样品进行苯并(a)芘添加回收试验,回收率为...     

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.     

Oxidative Stability of Soybean and Sesame Oil Mixture during Frying of Flour Dough

ABSTRACT: Effects of roasted sesame seed oil on the oxidative stability of soybean oil during frying of flour dough at 160 °C were studied by determining fatty acid composition and conjugated dienoic acid (CDA), p -anisidine (PA), and free fatty acid (FFA) values. Concentration of sesame oil in frying oil was 0%, 10%, 20%, or 30% (v/v). Tocopherols and lignan compounds in the frying oil were also determined by high-performance liquid chromatography. As the number of fryings performed by the oil increased, linolenic acid content in frying oil decreased, and the decreasing rate was lower in frying oil containing sesame oil than in the oil containing no sesame oil. CDA and FFA values of frying oil increased during frying and their relative values to the initial value were lower in frying oil containing sesame oil than in the oil containing no sesame oil. This indicates that the addition of sesame oil improved thermooxidative stability of frying oil, possibly due to the presence of lignan compounds in sesame oil. Tocopherols and lignan compounds in frying oil decreased during frying. As the amount of sesame oil in frying oil increased, degradation of tocopherols increased and lignan compounds degradation decreased. Tocopherols were suggested to protect lignan compounds in sesame oil from decomposition during frying.     

高效液相色谱在分析油脂成分方面的应用

综述了高效液相色谱在分析测定油脂成分方面的应用。主要是从高效液相色谱与不同的检测器联用测定各种油脂成分的方面进行阐述,并介绍了在检测餐饮废油脂中的应用。高效液相色谱在鉴别废油脂方面有着广阔的前景。     

发光杆菌SN259发酵液中二苯乙烯类化合物的分离、鉴定及体外抗氧化活性

为寻找高效天然的抗氧化剂,采用活性追踪法,利用固相萃取、柱层析、制备高效液相色谱等技术,对发光杆菌（Photohabdus temperata）SN259的发酵液进行分离纯化,得到9?个二烷基间苯二酚（dialkylresorcinols,DAR）衍生物类活性化合物,通过核磁共振和高效液相色谱-质谱综合解析和相关文献调研鉴定了所得活性化合物的结构,其中化合物1为新化合物,化合物2和3为首次分离纯化得到。对化合物1～9做抗氧化能力测试,并考察其对花生油氧化稳定性的影响,在2,2’-联氮-二(3-乙基-苯并噻唑-6-磺酸)阳离子自由基清除实验中,化合物1、8、9有较好的抗氧化能力,其自由基清除率达到50%时化合物的有效浓度分别为（4.95±0.11）、（6.17±0.09）、（4.55±0.07）μg/mL。     

Effects of Sesame Oil Addition to Soybean Oil During Frying on the Lipid Oxidative Stability and Antioxidants Contents of the Fried Products During Storage in the Dark

ABSTRACT: Effects of sesame oil addition to soybean oil during frying on the lipid oxidative stability and antioxidants contents of fried products during storage in the dark were studied. Flour dough pieces (2 cm × 2 cm × 0.1 cm) were fried at 160 °C for 1 min in sesame oil-added soybean oil. Concentrations of sesame oil in the frying oil were 0%, 10%, and 20% by volume. Fried products were put into a glass bottle, and the bottles were tightly sealed and stored at 60 °C in the dark for 18 d. Lipid oxidation of fried products was determined by fatty acid composition changes and conjugated dienoic acid (CDA) and p -anisidine (PA) values. Tocopherols and lignan compounds in the fried products were determined by high-performance liquid chromatography. Relative content of linolenic acid decreased, and CDA and PA values increased during storage of the fried products in the dark. Fatty acid composition change and CDA and PA values during storage were lower in the products fried in sesame oil-added soybean oil than in the products fried in soybean oil without sesame oil. The results clearly showed that addition of roasted sesame oil to soybean oil at 10% and 20% during frying decreased the lipid oxidation of fried products during storage in the dark for 18 d by extension of induction period and decrease in decomposition of oxidized lipids. Fried products contained 134 to 267 ppm tocopherols and 0 to 148 ppm lignans before storage; however, their contents decreased during storage in the dark. Lignan compounds were more stable than tocopherols, and the rate of tocopherols degradation was lower in the products fried in sesame oil-added soybean oil than in the products fried in soybean oil without sesame oil, which could be because of protection of tocopherols from degradation by lignan compounds.     

Application of triacylglycerol and fatty acid analyses to discriminate blended sesame oil with soybean oil

Triacylglycerols (TAGs) and fatty acids in the mixture of sesame oil (SO) with soybean oil were analysed using high performance liquid chromatography (HPLC)–an evaporative light scattering detector (ELSD) and gas chromatography (GC)–a flame ionisation detector (FID). Relative percentage of linolenic acid increased rapidly compared to those of oleic and linoleic acids as the ratio of soybean oil increased in the blended SO. Peak responses of trilinolein (LLL) and trilinolenin (LnLnLn) by HPLC–ELSD was higher than those by GC–FID from the same concentration of TAGs. The presence of LLLn peak, the contents of linolenic acid, and the relative ratio of L/S, O/Ln, and L/Ln from fatty acids or LLL/OOO from TAGs could be useful indicators to detect the blended SO with soybean oil. TAG analysis by HPLC–ELSD coupled with fatty acids by GC–FID can be useful methods to discriminate blended SO with soybean oil.