斑蝥炮制前后脂肪酸成分的GC-MS分析

目的:分析斑蝥炮制前后脂肪酸组成。方法:石油醚提取斑蝥脂肪油,甲酯化处理后采用气相色谱-质谱联用技术分析化合物组成,用峰面积归一化法确定各成分相对含量。结果:从炮制前后的斑蝥脂肪油中共分离鉴定出10种脂肪酸成分,脂肪酸组成以油酸、硬脂酸、亚油酸为主。结论:炮制对斑蝥脂肪酸组成影响不大。本试验可为斑蝥炮制前后的成分研究提供理论依据。     

鱼肝油中脂肪酸的气相色谱及气相色谱-质谱分析

目的 采用气相色谱法（GC）结合气相色谱-质谱（GC-MS）联用技术,对3种不同来源共26批鱼肝油样品中的脂肪酸成分进行测定。方法 通过氢氧化钾-甲醇碱催化法对鱼肝油样品进行甲基衍生化预处理,选用极性毛细管柱对样品中的衍生化产物脂肪酸甲酯进行分离,后经气相色谱仪-氢火焰离子化检测器（GC-FID）和气相色谱-质谱（GC-MS）联用仪进行分析检测。利用对照品定位法结合NIST谱库检索准确鉴定出棕榈酸、棕榈油酸、油酸、亚油酸、二十碳五烯酸（eicosapentaenoic acid,EPA）和二十二碳六烯酸（docosahexaenoic acid,DHA）等14种脂肪酸,并通过面积归一化法对这14种脂肪酸进行定量分析。结果 这14种脂肪酸在国内鱼肝油中的含量与模拟天然鱼肝油和进口鱼肝油样品中的含量存在较大差异。其中,EPA和DHA等脂肪酸在模拟天然鱼肝油和进口鱼肝油样品中的含量远高于其在国内鱼肝油样品中的含量,而亚油酸在国内鱼肝油样品中的含量却高达44%以上,10倍于其在另外2种鱼肝油样品中的含量。结论 不同来源的鱼肝油样品中的脂肪酸成分不尽相同,可根据脂肪酸的组成区别鱼肝油样品中是否添加天然鱼肝油成分。     

Formyl-methionyl-leucyl-phenylalanine and a calcium ionophore A23187 reverse the inhibition of phorbol myristate acetate-induced oxidative burst by linoleic and oleic acid anilides

Linoleic and oleic acid anilides profoundly inhibited the production of reactive oxygen metabolites (ROM) in human polymorphonuclear leukocytes (PMNL) induced by a tumor promoter, phorbol myristate acetate (PMA). The addition of a Ca²⁺ ionophore, A23187, or a chemotactic peptide, formyl-methionyl-leucyl-phenylalanine (fMLP), readily reversed linoleic and oleic acid anilide-induced inhibition of PMA-evoked respiratory burst in PMNL without affecting PMA-induced respiratory burst. fMLP or A23187 caused a marked increase in the production of ROM in PMNL that did not produce ROM after their co-exposure to PMA and cis-fatty acid anilides. This suggests a role for Ca²⁺ in this restoration of respiratory burst activity in PMNL. Oleic and linoleic acid anilides enhanced also respiratory burst in PMNL subsequent to their stimulation with fMLP. Interestingly, corresponding fatty acids, linoleic and oleic acid, also inhibited PMA-induced production of ROM in PMNL, but this inhibition was not reversed by A23187 or fMLP. These findings suggest that the aniline moiety of cis-fatty acids significantly modifies the effects of linoleic and oleic acids in the production of ROM in PMNL. Moreover, free intracellular Ca²⁺ may play a critical role in the activation of PMNL to produce ROM, and in the modulation of the effects of cis-fatty acid anilides.     

柱前衍生化HPLC法测定百多宁注射液中的脂肪酸含量

目的建立以HPLC法测定百多宁注射液中脂肪酸含量的方法。方法采用无水硫酸钠破乳方法分离百多宁注射液中的油相。以 2 ,4′ 二溴苯乙酮为衍生化试剂 ,18-冠 - 6醚为相转移催化剂 ,采用C8反相柱 ,以乙腈 -水 (V∶V =75∶2 5 )为流动相等度洗脱 ,正十七烷酸为内标 ,一次基线分离 4种脂肪酸。结果亚油酸在 4 6～ 30 7ng内、软脂酸在 2 7 2～ 181 0ng内、油酸在 14 4～96 0ng 内、硬脂酸在 9 7～ 6 5 1ng内质量与相对峰面积线性关系良好 ,相关系数分别为 0 9997、0 9999、0 9995、0 9996。平均回收率分别为 98 2 %、97 5 %、99 8%、10 2 3% ,RSD分别为2 6 %、3 0 %、1 2 %、2 4 %。结论方法重现性好、定量准确 ,可作为百多宁注射液中脂肪酸测定的定量方法     

蚕蛹油α-亚麻酸提取工艺研究和成分分析

目的研究筛选从蚕蛹油中提取α 亚麻酸的工艺路线 ,并对提取的不饱和脂肪酸进行成分分析。方法采用酸水解法、碱水解法和皂化法等三种工艺方法 ,以新鲜蚕蛹为原料制备蚕蛹油 ,并用气相色谱仪对所得蚕蛹油进行成分分析。结果三种工艺方法制备蚕蛹油中不饱和脂肪酸含量分别为 5.2 6%、3 .0 4%及 5.51% ,表明蚕蛹油中含有丰富的不饱和脂肪酸 ;蚕蛹油不饱和脂肪酸中亚油酸、油酸、α 亚麻酸的含量分别为 3 7.53 % ,4.94%及3 0 .2 4%。结论皂化法工艺提取蚕蛹油不饱和脂肪酸收率较高 ,且进一步分离蚕蛹油不饱和脂肪酸中α 亚麻酸有较好的应用前景     

白芍和赤芍成分的比较

芍药为我国原产,栽培的历史极久,其根供药用,亦有悠久的历史。神农本草经列为中品,主治“邪气腹痛除血痹破坚积寒热疝瘕止痛利小便益气”。陶宏景谓:“今出白山蒋山茅山最好白而长尺许余处亦有而多赤赤者小利。”雷公炮炙论称:“凡采用竹刀刮去皮并头上剉细以蜜水伴蒸从已至未晒于是为白芍。”纲目又称:“今人多生用唯避中寒者以酒炒。入女人血药以醋炒耳。”若采得直接晒干供用的是为赤芍。所以后世将芍药分为白芍和赤芍二种,至今仍旧沿用。供药用的芍药原为野生品,后渐用栽培的。现代中     

On the generation and outcome of 3-(N-phenylamino)propane-1,2-diol derivatives in deodorized model oils related to toxic oil syndrome

Toxic Oil Syndrome (TOS) was a massive food-born intoxication that occurred in Spain in 1981 and affected more than 20,000 people. TOS was attributed to the ingestion of rapeseed oil that had been adulterated with aniline, illegally refined, and delivered for human consumption. Two chemical species derived from aniline have been identified in oil batches: fatty acid anilides, qualified as biomarkers of the adulterated oil, and fatty acid esters of 3-(N-phenylamino)propane-1,2-diol (PAP), considered toxic oil biomarkers. These esters were generated by chemical processes during oil refining, specifically in the deodorization step, which involves treatment of the oil at high temperatures under vacuum to remove volatile contaminants. Since PAP derivatives are strongly associated with TOS, their formation and putative interconversion in a toxic oil model has been studied. The main results obtained are (i) only triglycerides and aniline are required to produce PAP esters, thus eliminating the possibility that unknown activators present in the deodorization tank were required for toxification of the oil; (ii) PAP and PAP mono- and diesters are chemically interrelated, as are anilides and PAP esters to an even higher degree. In addition to the reaction of aniline with triglycerides, anilides can be also formed via attack of PAP esters by aniline. However, the most important source of anilides during deodorization seems to be the thermal decomposition of PAP esters. Overall, these results suggest that the generation and outcome of PAP derivatives during deodorization is a complex scenario whereby PAP esters are not only generated from different reactions but decompose to produce anilides, among other compounds. In addition to providing a rapeseed oil model that reproduces the composition of case oils with respect to anilides and PAP derivatives, the results presented herein further support the hypothesis imputing PAP diesters or their metabolites for the intoxication episode.     

Storage time and deodorization temperature influence the formation of aniline-derived compounds in denatured rapeseed oils.

In 1981 an epidemic, named Toxic Oil Syndrome, occurred in Spain as a result of ingestion of rapeseed oil denatured with 2% aniline, which had been imported for industrial use but was fraudulently diverted and processed for human consumption. Two groups of chemical compounds have been identified in the ingested toxic oil: fatty acid anilides and amino-propanediol derivatives. The objective of this work was to assess the effect of several refining process variables on the formation of 3-(N-phenylamino)-1,2-propanediol (PAP) esters. The amount of PAP esters in aniline-denatured oil increased dramatically when oil was heated from 250 degrees C to 300 degrees C. However, the ones formed when 300 degrees C was reached were lost during processing at that temperature. The level maintained during the operation time at 300 degrees C was higher in denatured samples stored for 3 weeks before refining than in denatured samples stored only for 1 week. Anilides were also analyzed. We found that anilides decreased very little with distillation time. In this paper we discuss the influence of storage time prior to refining and of elevated refining temperature, such as temperatures that might occur in close proximity to a deodorizer coil.     

酸藤子脂肪酸类成分的GC-MS研究

目的:研究酸藤子的脂肪酸类成分。方法:酸藤子根部以95%乙醇提取,用石油醚对提取物进行萃取,所得萃取部位经甲酯化处理后,采用气相色谱-质谱(GC-MS)联用技术进行分析鉴定;酸藤子枝叶用石油醚提取,所得提取物也用GC-MS联用技术进行分析鉴定。再用峰面积归一化法测定各成分的相对含量。结果:酸藤子根部共分离出67个色谱峰,鉴定了其中28个,占流出峰总面积的73.48%,主要脂肪酸成分为8,11-亚油酸(19.10%)、8-油酸(13.01%)与棕榈酸(12.29%)。酸藤子枝叶共分离出30个色谱峰,鉴定了其中12个,占流出峰总面积的91.60%,主要脂肪酸成分为棕榈酸(52.16%)。结论:酸藤子根部和枝叶的脂肪酸类成分有差异。本试验结果可为酸藤子的深入开发提供一定的科学依据。     

用石油醚代替乙醚检测食油中的酸价

目的探讨检测食品中油脂酸价的方法。方法用石油醚代替乙醚测定食品油脂中的酸价与国标法比较,进行统计分析,探讨是否存在差异。结果用石油醚代替乙醚测定食品油脂中的酸价与国标法相比较,测定值经统计分析结果无显著性差异。结论用本法可以进行食品中酸价的测定,减少对人的危害,体现以人为本的精神,结果准确可靠。     

蒼耳油中主要不饱和脂肪酸的研究

本文报道了从苍耳油制备亚油酸的一种尿素-锂盐合并的新方法.采用本法,所得亚油酸,收率特高(40%)质量亦好(98.6%).此外,还可回收一部分油酸.重复试验的结果,证明新法较之常用的方法为佳.     

柑桔籽油中脂肪酸的GC/MS分析

应用超临界CO2萃取柑桔籽油,经GC/M S联用技术分离鉴定出9种脂肪酸,其中亚油酸占44.1%,油酸占24.1%,不饱和脂肪酸达73.41%。     

牵牛子脂肪油超临界CO_2萃取及气相-质谱测定

目的 :提取分析牵牛子脂肪油及其成分。方法 :用超临界CO2 萃取法提取牵牛子脂肪油 ,结合气相 -质谱法分析脂肪油成分。结果 :牵牛子脂肪油含量为34.78% ,脂肪酸组成以亚油酸、油酸和棕榈酸为主 ,不饱和脂肪酸占脂肪酸总量的88.70% ,饱和脂肪酸以棕榈酸为主。结论 :牵牛子脂肪油属优质植物油,分析结果可为开发、利用牵牛子油脂资源提供科学依据     

超临界流体CO_2萃取使君子仁脂肪油化学成分的研究

目的:分析使君子仁脂肪油含量及其脂肪酸组成。方法:以超临界流体CO2萃取使君子仁脂肪油,采用重量法和气相色谱-质谱联用技术分别测定油含量和脂肪酸组成。结果:使君子仁脂肪油含量为27.70％,脂肪酸组成以油酸、亚油酸和棕榈酸为主,不饱和脂肪酸占脂肪酸总量的63.93％,饱和脂肪酸以棕榈酸为主。结论:使君子仁脂肪油属优质植物油,分析结果可为其开发利用提供科学依据。     

椒目仁油与5种食用油中5种脂肪酸的含量比较

目的:建立测定椒目仁油与紫苏油、花生油、菜籽油、大豆油、山茶油中棕榈酸、硬脂酸、油酸、亚油酸与α-亚麻酸含量的方法,并对上述6种植物油中5种脂肪酸的含量进行比较。方法:采用十四酸作为内标,先甲酯化脂肪酸,再用气相色谱法测定5种脂肪酸的含量。色谱柱为涂布浓度15%丁二酸二乙二醇聚酯的不锈钢填充柱(2000mm×3mm),柱温为180℃,进样口温度为300℃,检测器为氢火焰离子化检测器,检测器温度为320℃,载气为高纯氮,流量为40mL·min-1,不分流进样。结果:6种植物油中棕榈酸、硬脂酸、油酸、亚油酸、α-亚麻酸及总的不饱和脂肪酸含量,椒目仁油中分别为10.79%、2.93%、19.36%、27.73%、31.61%、78.70%,紫苏油中分别为7.74%、4.29%、17.04%、10.34%、58.64%、86.02%,花生油中分别为4.10%、3.59%、41.92%、32.21%、0.24%、74.37%,菜籽油中分别为2.52%、1.51%、22.88%、41.76%、8.03%、72.67%,大豆油中分别为13.84%、4.98%、19.32%、45.12%、6.28%、70.72%,山茶油中分别为5.17%、3.75%、37.46%、3.82%、0.26%、41.54%。结论:椒目仁油与其余几种油比较具有不饱和脂肪酸含量高、来源丰富、制作简单、价格便宜等优点,可以作为补充脂肪酸的来源。     

双边栝蒌种子油含量及其脂肪酸的测定

目的：测定双边栝蒌种子油的含量及其脂肪酸组成。方法：用重量法和GC-MS法测定。结果：双边栝蒌种子油含量为31.24%，脂肪酸组成以亚油酸和油酸为主，不饱和脂肪酸占脂肪酸总量的90.48%,饱和脂肪酸以棕榈酸和硬脂酸为主。结论：双边栝篓种子油属优质植物油，可作为油脂资源开发利用。     

GC/MS分析紫苏子与亚麻子脂肪酸成分

探讨紫苏子和亚麻子油中的脂肪酸组成,为开发利用提供依据。方法：化学法萃取紫苏子和亚麻子油,ＧＣ／ＭＳ分析油中的脂肪酸成分。结果：紫苏子和亚麻子得油率（Ｗ／Ｗ）分别为２９．５２％和３８．９７％。紫苏子油中检出软脂酸、亚油酸、α－亚麻酸、硬脂酸、二十碳—烯酸和二十碳烷酸等６种脂肪酸,它们的相对百分含量分别为５．９１％、７．０３％、８４．５０％、２．４１％、０．０５％和０．１０％;亚麻子油中检出软脂酸、亚油酸、α－亚麻酸、硬脂酸和二十二碳烷酸等５种脂肪酸和２种未知成分,已知脂肪酸成分占总脂肪酸组分的９９．９１％,其相对百分含量分别为４．２９％、８．２０％、８３．８４％、３．５３％和０．０５％。结论：紫苏子和亚麻子油的脂肪酸组成均比较简单,并富含可开发利用的α－亚麻酸。     

萃取-显色法快速测定莪术油脂质体包封率

目的：建立快速测定莪术油脂质体（ZTO-L）包封率的方法。方法：采用香草醛硫酸显色法,在波长520nm处测定脂质体中莪术醇的含量,利用石油醚萃取法分离ZTO-L与游离药物,考察石油醚用量与脂质体和药物回收率的关系;并与葡聚糖凝胶柱色谱分离法和透析法进行比较。结果：莪术醇浓度在0.8～6.0μg·ml-1线性关系良好（r=0.997）。莪术油中莪术醇的百分含量为70.37%。石油醚萃取法对空白脂质体的回收率为99.34%,对莪术醇回收率为98.77%,用该法所测脂质体平均包封率为70.78%。透析法不适合用于分离ZTO-L与游离药物。结论：萃取-显色法可快速准确地测定ZTO-L的包封率,且不受脂质体粒径、ZETA电位的限制。     

Effects of various vehicles and fatty acids on the skin permeation of lornoxicam

Transdermal permeation of lornoxicam, one of potent non-steroidal anti-inflammatory drugs, was studied in vitro with various vehicles and fatty acids using hairless mouse dorsal skin and human cadaver full skin. Vehicles used were diethylene glycol monoethyl ether (DGME), propylene glycol monocaprylate, propylene glycol, oleyl alcohol, dimethyl sulfoxide (DMSO) and others. Various fatty acids were employed as enhancers. Among pure vehicles studied, only DMSO showed permeation from saturated solutions. In the case of DMSO?CDGME co-solvent, the higher the DGME ratios were, the lower the fluxes were. The addition of fatty acid (3?w/v?%) increased the permeation in the rank order of linoleic acid (LOA)????oleic acid????lauric acid?>?capric acid?>?caprylic acid. Enhancement ratios ranged from 2 to 37 compared to the flux without fatty acid. Lornoxicam flux decreased in inverse proportion to the concentration of triethanolamine (TEA), which was used as a salt former and solubilizer. However, the flux increased linearly as the donor dose increased even in the presence of TEA. Using human cadaver skin, the permeability of lornoxicam was much lower than that using the hairless mouse skin, but fluxes increased as the concentration of LOA increased. These results indicate the feasibility of lornoxicam transdermal delivery with a combination of fatty acid and TEA in DMSO or DMSO?CDGME cosolvents.     

Free radical scavenging and tyrosinase inhibition activity of oils and sericin extracted from Thai native silkworms (Bombyx mori)

Oils and sericin were extracted from pupae and silk cocoons, respectively, of the five Thai native silkworms (Bombyx mori, Linnaeus (Bombycidae)), namely, Keawsakol, Nangnoi, Somrong, Nangleung, and Noneruesee, which are variations of the same species. The oils were extracted by a hot process using Soxhlet apparatus and a cold process using petroleum ether, while sericin was extracted by basic hydrolysis and autoclaving. Sericin from the five Thai native silkworms showed free radical scavenging activity lower than the standard antioxidants (vitamin C, vitamin E, and BHT) by about 20–100-fold, but all oils gave higher activity than that of the standard linoleic acid by 11–22-fold. Oil extracted from Noneruesee by the cold process gave the highest DPPH scavenging activity, compared with other oil samples. All sericin samples showed tyrosinase inhibition activity with IC₅₀ values in the range of 1.2–18.76?mg/mL, but only oils from Noneruesee extracted by the hot process, and Nangleung, Somrong, and Noneruesee extracted by the cold process, showed this activity. Oil extracted by the hot process and sericin by basic hydrolysis from Noneruesee gave the highest tyrosinase inhibition activity, but lower than that of the standards vitamin C and kojic acid by 20–49 and 3–8 times, respectively. This study has suggested that sericin and oil from Noneruesee extracted by basic hydrolysis and the cold process, which gave the highest tyrosinase inhibition and free radical scavenging activity, respectively, can be applied in antiaging and whitening cosmetic products.