不同蜂花粉中磷脂成分的比较

采用薄层色谱、高效液相色谱分离测定蜂花粉中磷脂,并分析磷脂中不饱和脂肪酸的含量。结果表明：茶花、葵花、玫瑰、籽瓜、益母草蜂花粉中富含磷脂,其中茶花蜂花粉中总磷脂含量最高,主要由磷脂酰肌醇、磷脂酰丝氨酸、磷脂酰乙醇胺、磷脂酰胆碱及溶血卵磷脂组成;脂肪酸组成分析表明,蜂花粉中磷脂多不饱和脂肪酸含有较高含量的亚油酸和亚麻酸,5种蜂花粉磷脂中多不饱和脂肪酸含量均在50%以上,其中茶花蜂花粉磷脂中亚麻酸在脂肪酸含量中最高达56.0%。蜂花粉中多元不饱和磷脂具有广阔的开发前景。     

柱层析法分离大豆磷脂

通过实验探讨了使用低压制备色谱柱在等度洗脱方式下分离大豆磷脂中的磷脂酰肌醇(PI)、磷脂酰乙醇胺(PE)、磷脂酰胆碱(PC)等成分.结果表明,在使用100cm×26 mm规格的色谱柱、氯仿-甲醇(2∶1)作为流动相、流速控制在3.0 mL/min,负载量为0.25 g/150 g硅胶(100～200目)的条件下可以分离得到PI纯度在90%以上、PE纯度在80%以上、PC纯度在95%以上的各种产品.     

卵磷脂类保健食品中PE、PC的高效液相色谱测定

为准确快速地对卵磷脂保健食品中有效成分进行定量分析 ,我们建立了卵磷脂保健食品中磷脂主要组分磷脂酰胆碱 (PC)、磷脂酰乙醇胺 (PE)的高效液相色谱测定方法。方法的日间精密度为 5 4 %～ 9 0 %;PE、PC的加标回收率分别为 83 0 %～ 10 5 6 %和 81 3%～ 86 0 %,均可满足卫生分析的要求。对 5种卵磷脂保健食品中的PC、PE的含量进行了测定 ,PC、PE的含量分别为15 2 %～ 2 4 2 %和 3 1%～ 6 1%。方法的样品前处理方法简单 ,且检测灵敏度高 ,分析速度快 ,适于在国内推广使用     

核磁共振氢谱法测定卵磷脂、溶血磷脂和甘油磷脂酰胆碱含量

利用核磁共振氢谱测定磷脂酶A1催化水解大豆卵磷脂后的样品中卵磷脂(PC)、溶血磷脂(LPC)、甘油磷脂酰胆碱(GPC)的相对含量。分别选取化学位移δ=4.40~4.50、4.14~4.16、3.76~3.83处的信号峰作为PC、LPC和GPC的特征性质子峰,并根据质子峰相对面积与物质的量的对应关系计算三者的相对含量。结果表明,PC、LPC、GPC的加标回收率分别为101.6%~107.0%、79.8%~92.4%、102.0%~107.1%,相对标准偏差(RSD)分别为1.6%~2.5%、3.6%~6.5%、5.6%~6.7%;精密度试验中PC、LPC、GPC的RSD分别为4.2%、3.5%、2.3%;对磷脂酶A1催化水解大豆卵磷脂4 h与8 h的两个样品进行检测,结果表明样品中PC、LPC、GPC的相对含量分别为71.2%、22.1%、6.7%;22.4%、0、77.6%。     

养殖大黄鱼各部位磷脂组分及其脂肪酸组成分析

为明确大黄鱼各部位磷脂组分及其脂肪酸组成,本实验选取大黄鱼头部、背肌、腹肌、内脏、尾部以及鱼卵为研究对象,分别测定各部位的磷脂含量、组分及其脂肪酸组成。结果表明:鱼卵中磷脂含量最高,为5.50 g/100 g。头部、背肌和腹肌磷脂组分一致,为溶血磷脂酰胆碱(LPC)和磷脂酰胆碱(PC);头部磷脂中LPC和PC的含量分别为39.23%、45.12%,背部分别为62.74%、36.12%,腹部分别为66.69%、33.31%。内脏磷脂组分为溶血磷脂酰胆碱(LPC)、磷脂酰肌醇(PI)和鞘氨醇磷脂(SM),含量分别为59.37%、12.77%、29.83%。鱼尾磷脂为LPC、PC和磷脂酰乙醇胺(PE),含量分别为21.41%、59.37%、19.22%。鱼卵磷脂为LPC、PI、PE和PC,含量分别为12.30%、1.09%、9.12%、76.36%。脂肪酸组成分析表明大黄鱼各部位富含多不饱和脂肪酸,其中鱼卵磷脂中多不饱和脂肪酸占比43.1%,明显优于大黄鱼其他各部位。研究结果说明大黄鱼是一种富含磷脂功能因子的海洋鱼类。     

哈维氏弧菌磷脂酶D对不同磷脂单分子层的吸附动力学研究

基于单分子层技术研究了哈维氏弧菌来源磷脂酶D(Vh PLD)对不同磷脂单分子层的吸附动力学。探究初始表面压力条件对VhPLD吸附不同磷脂单分子层(磷脂酰胆碱(PC)、磷脂酰乙醇胺(PE)、磷脂酰丝氨酸(PS)、磷脂酰甘油(PG)和磷脂酰肌醇(PI))吸附动力学参数(k_a、k_d、K_(Ads))的影响规律。结果表明:VhPLD对磷脂单分子层的吸附动力学参数与磷脂单分子层初始表面压力密切相关;在15 m N/m条件下,VhPLD对不同磷脂单分子层吸附偏好性顺序为PC PG PS PE=PI;在20 m N/m条件下,VhPLD对不同磷脂单分子层吸附偏好性顺序为PG PI PC PS PE;在25 m N/m条件下,VhPLD对不同磷脂单分子层吸附偏好性顺序则转变为PC PS PI PE=PG。     

人乳的磷脂组成与脂肪球结构

采用核磁共振磷谱(~(31)P-NMR)测定不同泌乳期、不同胎龄的人乳磷脂组成,结果显示足月儿和早产儿人乳中,磷脂的主要组成均为鞘磷脂(SM)、磷脂酰胆碱(PC)、磷脂酰乙醇胺(PE)、磷脂酰乙醇胺缩醛磷脂(EPLAS)、磷脂酰肌醇(PI)和磷脂酰丝氨酸(PS),其中SM含量最高,其次为PC和PE,PS和PI含量最低。总磷脂含量在相同胎龄不同泌乳期以及相同泌乳期不同胎龄间均无显著性差异。在磷脂组成上,足月儿人乳中PI在初乳和过渡乳中的含量分别为(4.14±0.42)%和(3.66±0.66)%,显著高于成熟乳中的(2.79±0.09)%;早产儿人乳中PC在初乳和过渡乳中的含量分别为(30.74±2.03)%和(29.40±2.37)%,显著高于成熟乳的(27.55±2.42)%,此外EPLAS含量随泌乳期的延长逐渐降低,PE含量逐渐升高,PE+EPLAS在不同的泌乳期无显著性差异。另外,足月儿和早产儿的脂肪球结构无明显差异,磷脂构成的膜包裹体积平均粒径约为5μm的脂肪球。     

UPLC-Triple-TOF-MS/MS法分析中国东北地区人乳磷脂的组成

借助超高效液相色谱联用质谱(UPLC-Triple-TOF-MS/MS)分析法,对不同泌乳期人乳中的磷脂进行定性和相对定量,为中国人乳磷脂组成的研究提供参考。本研究从哈尔滨(黑龙江省)、齐齐哈尔(黑龙江省)和吉林(吉林省)地区采集到汉族人初乳(1~5 d)、过渡乳(6~20 d)和成熟乳(21 d~)共计73份。LipidView 1.2用于检索磷脂分子式,PeakView 2.2及其插件MasterView 1.1用于磷脂定性分析,MultiQuant用于磷脂相对定量分析(基于色谱峰面积)。结果显示,人乳中检出磷脂共计60种。其中,磷脂酰胆碱(PC)17种,磷脂酰乙醇胺(PE)25种,磷脂酰丝氨酸(PS)4种,磷脂酰肌醇(PI)5种,鞘磷脂(SM)9种。磷脂酰胆碱(PC)、磷脂酰乙醇胺(PE)、鞘磷脂(SM)、磷脂酰丝氨酸(PS)和磷脂酰肌醇(PI)在总磷脂中的相对含量分别为38.12%、26.97%、29.54%、4.43%和0.94%,各种磷脂的相对含量随泌乳期变化表现出不同的变化趋势,但大多数磷脂的相对含量差异并不显著。     

高效液相色谱法测定磷脂软胶囊中磷脂酰胆碱、磷脂酰肌醇、磷脂酰乙醇胺的含量

目的建立高效液相色谱法同时检测磷脂软胶囊中磷脂酰胆碱(phosphatidyl cholines, PC),磷脂酰乙醇胺(phosphatidyl ethanolamine, PE),磷脂酰肌醇(phosphatidylinositol, PI)3种组分的含量。方法样品用甲醇超声提取后,经Bridge?HILIC色谱柱(4.6 mm×150 mm, 5μm)分离,以0.9 mmol/L甲酸铵溶液-乙腈为流动相进行梯度洗脱,流速为1.0 mL/min;柱温30℃;检测波长为205 nm,外标法定量。结果磷脂酰胆碱,磷脂酰乙醇胺,磷脂酰肌醇在浓度0.025～0.250mg/mL范围内线性关系良好,相关系数均大于0.99,检出限分为0.300～1.386 mg/g,定量限为1.002～4.624 mg/g,加标回收率分别为90%～105%,相对标准偏差为1.0%～4.0%。结论该方法高效,便捷,准确度高,适用于磷脂软胶囊中3种磷脂成分的同时检测。     

卵磷脂保健食品中磷脂酰胆碱的含量测定

建立一种准确、快速的对卵磷脂保健食品中的主要组分磷脂酰胆碱(PC)进行定量分析的方法。采用紫外分光光度法，将卵磷脂的正己烷提取液与0．5％碘-正己烷溶液反应后，292nm波长处测定吸光度。吸光度与磷脂酰胆碱的含量呈线性相关，吸光值在0．35-1．1范围内线性关系良好，相关系数为0．9994。本方法准确、快速，简便，适于卵磷脂保健食品中磷脂酰胆碱的含量测定。     

Phospholipid changes in the course of beef meat storing at 4 °C

The mean molecular weight of beef meat phospholipids (738) and the recalculating factor (23.8), making possible to determine the total phospholipid content from lipid phosphorus, were estimated experimentally. The total amount of phospholipids decreases from 569 to 486 mg per 100 g of meat during 14 days of meat storing at 4 °C. The content of phosphatidylcholine, sphingomyelin, phosphatidylserine and phosphatidylinositol decreases, too. In contrast to this the content of lyso-phosphatides and temporarily also phosphatidylethanolamine is increasing. This temporary increase of phosphatidyiethanolamine (PE) concentration is due to enzymatic demethylation of phosphatidylcholine (PC). The course of this conversion has been followed by PE PC ratio changes in the course of meat storing.     

Flavonoids as biochemical markers of the plant origin of bee pollen

The flavonoid compounds present in almond (Prunus amygdalus, Rosaceae), Jara (Cistus sp Cistaceae), Echium sp (Boraginaceae) and Chrysanthemum sp (Compositae) bee pollens have been studied by TLC, 2D PC and HPLC techniques. These bee pollens show characteristic flavonoid patterns which allow their use as biochemical markers of their plant origin. In addition, the flavonoid patterns of natural almond and ?Jara’? pollens have been shown to be identical to those of the corresponding bee pollens confirming their use as chemical markers. The flavonoid aglycones obtained by acid hydrolysis of pollen flavonoids are also useful for identification purposes. Almond bee pollen contains 8-methoxykaempferol, kaempferol and quercetin 3-glycosides, ?Jara’? bee pollen produces quercetin and isorhamnetin 3-glycosides and trace amounts of myricetin and kaempferol 3-glycosides, Echium bee pollen contains mostly kaempferol 3-glycosides and traces of quercetin 3-glycosides, and Chrysanthemum contains kaempferol, apigenin, and quercetin 3-glycosides. The major compound in almond pollen, namely 8-methoxykaempferol 3-glycoside, was not detected in the related apple, pear, cherry and plum pollens.     

基于斑马鱼模型研究不同磷脂促血管生成活性

目的：利用斑马鱼模型研究不同来源和不同类型的磷脂对血管生成的促进作用及其活性差异。方法：将受精后发育24 h和72 h的斑马鱼胚胎脱膜,分别用于评估各磷脂样品（分别以大豆、蛋黄和南美白对虾虾头制备）对斑马鱼体节间血管（intersegmental vessel,ISV）和肠下静脉（subintestinal vein vessel,SIV）生长情况的影响,设置空白对照组、模型组（0.25 μg/mL PTK787）、阳性对照组和磷脂样品组（20、40、80 mg/mL）,给药24 h后用荧光显微镜观察并记录各实验组转基因斑马鱼ISV和SIV的生长情况。结果：对于ISV受损斑马鱼而言,3 种磷脂提取物以及2 种磷脂市售产品（药品和保健品）均表现出明显的血管生成促进作用,对于SIV而言,3 种磷脂提取物以及4 种磷脂市售产品（药品和保健品）均表现出明显的血管生成促进作用,相对而言,南美白对虾虾头磷脂促进血管生成活性更强,效果更加明显;5 种磷脂标准品表现出不同程度的血管生成促进作用,对于ISV受损斑马鱼而言,磷脂酰乙醇胺、磷脂酰胆碱、磷脂酰丝氨酸以及高质量浓度（80 mg/mL）的鞘磷脂表现出明显的促血管生成作用,对于SIV受损斑马鱼而言,所有的磷脂标准品均表现出较明显的血管生成促进作用。结论：不同质量浓度的磷脂提取物、市售产品以及磷脂标准品对斑马鱼均具有一定的促血管生成活性。     

六种鱼鱼头磷脂的组成及脂质脂肪酸分析

为研究海水鱼和淡水鱼鱼头磷脂及脂质脂肪酸组成的差异,以海水鱼(马鲛鱼、巴浪鱼、金鲳鱼)和淡水鱼(罗非鱼、鲫鱼、鲢鱼)鱼头为研究对象,利用Floch法提取6种鱼鱼头总脂;硅胶柱层析法将总脂分离收集中性脂、糖脂和磷脂;薄层层析(thin layer chromatography,TLC)分析比较6种鱼鱼头磷脂种类的分布、组成;气相色谱(Gas chromatography,GC)分析6种鱼鱼头脂质的脂肪酸组成。结果表明,6种鱼鱼头中提取率最高的脂质类型为中性脂,占总脂的48.98%~77.84%,其次为磷脂,占总脂的5.93%~22.86%,糖脂提取率最低,占总脂的3.67%~15.91%。鱼头磷脂中共检出4种磷脂组分,分别为磷脂酰乙醇胺(Phosphatidylethanolamine,PE)、磷脂酰胆碱(Phosphatidylcholine,PC)、鞘磷脂(Sphingomyelin,SM)、溶血磷脂酰胆碱(Lysophosphatidylcholine,LPC),其中PC明显高于其他磷脂组分。脂质中均含有较高含量的多不饱和脂肪酸(Poly-unsaturated fatty acid,PUFA),其中以二十二碳六烯酸(docosahexaenoic acid,DHA)为主,且均含有二十碳五烯酸(eicosapntemacnioc acid,EPA),海水鱼和淡水鱼鱼头磷脂中DHA和EPA占总脂肪酸的比例最高,分别为18.39%~21.43%和5.61%~10.38%,且海水鱼鱼头中以DHA和EPA为主的PUFA含量高于淡水鱼鱼头。因此,海水鱼鱼头是提取n-3多不饱和脂肪酸的潜在资源,尤其是制备n-3多不饱和脂肪酸型磷脂的良好来源。     

大黄鱼鱼卵磷脂对小鼠脂质代谢的调节作用

为研究大黄鱼鱼卵磷脂对高脂血症小鼠降血脂作用的影响,通过建立高脂血症小鼠模型,随机分为模型组、空白组、大豆磷脂组以及大黄鱼鱼卵磷脂低(5 g/kg)、中(15 g/kg)和高剂量组(30 g/kg),连续饲料喂养4周后,测定血清相关指标,并进行肝脏病理观察。结果表明:大黄鱼鱼卵磷脂具有抑制小鼠体重增加的作用。血清指标数据分析显示,与模型组相比,大黄鱼鱼卵磷脂低剂量组可显著降低TC、TG水平及AI_1、AI_2值(p0.05),对降低LDL-C和提高HDL-C水平差异不显著,而中和高剂量组均能显著降低TC、TG和LDL-C水平以及AI_1、AI_2值,可以显著提高HDL-C水平(p0.05),表明大黄鱼鱼卵磷脂具有调节高脂血症小鼠脂质代谢的作用;小鼠肝脏病理组织学观察显示,大黄鱼鱼卵磷脂低剂量组对小鼠肝细胞无明显影响,而中和高剂量组可以明显修复小鼠肝细胞变性。结果提示大黄鱼鱼卵磷脂可预防小鼠肝脏的脂肪性病变,有助于降低动脉粥样硬化发生的风险。     

利用高效液相色谱-蒸发光检测器法分析鮰鱼脑中磷脂组成

对鮰鱼脑中的磷脂进行提取纯化,利用高效液相色谱-蒸发光检测器法对鮰鱼脑的磷脂含量进行检测。结果表明：鮰鱼脑磷脂中磷脂酰胆碱含量最高,占磷脂含量的45.73%,磷脂酰乙醇胺次之,含量为17.39%,磷脂酰丝氨酸含量为5.01%,磷脂酰肌醇含量为1.20%,相对较低。磷脂标准品在各自的质量浓度检测范围内线性关系良好,并且鮰鱼脑的磷脂中各组分分离效果良好,对于其他磷脂样品的测定也具有重要的参考价值。     

Simultaneous Determination of Organochlorine, Organophosphorus, and Pyrethroid Pesticides in Bee Pollens by Solid-Phase Extraction Cleanup Followed by Gas Chromatography Using Electron-Capture Detector

A method for routine determination of the residues of nine organochlorine pesticides (OCPs), ten organophosphorus pesticides (OPPs), and seven pyrethroid pesticides (PPs) in bee pollens was developed. Bee pollen samples were extracted by petroleum ether followed by solid-phase extraction cleaning and detected by gas chromatography–micro electron capture detection. Range of detection limits are 0.3–3.3 μg/kg for OCPs, 1.0–19.1 μg/kg for PPs and 1.1–19.7 μg/kg for OPPs. Recoveries of OCPs, OPPs, and PPs were in the range of 88.9–122.7 %, 86.8–123.1 %, and 90.8–118.7 %, respectively. The method was applied successfully to analyze real bee pollen samples. The results show a low level of contamination caused by pesticide residues indicating safe supply of bee pollen for consumers.     

Phospholipids determination in vegetable oil by thin-layer chromatography and imaging densitometry

A rapid reliable method was developed to measure vegetable oil phospholipid content by thin-layer chromatography–imaging densitometry. Phospholipid samples were obtained from crude soybean oil by water degumming and then analyzed and quantified by thin-layer chromatography and imaging densitometry. Phosphatidyl choline (PC), phosphatidyl ethanolamine (PE) and phosphatidyl inositol (PI) standard curves were generated. The total phospholipid content of the oil was 1.12–1.26%, of which 27.1 ± 1.86% was PC, 22.7 ± 0.45% was PE, while PI accounted for 17.2 ± 0.85% of the total. A high correlation coefficient of 0.985 was found for reproducibility of pixel area (OD*mm) at a constant concentration of standard phospholipid. Regression analysis of the pixel area vs the phospholipid (PC, PE, and PI) weights (μg) generated R² greater than 0.983. Thin-layer chromatography–imaging densitometry proved a useful tool for rapid determination and quantification of the major phospholipids in soybean oil.     

Seasonal changes in phospholipids of mussel (Mytilus edulis Linne)

The phospholipids of mussels (Mytilus edulis Linne) from the coast of Qingdao were extracted, fractionated and analysed over a 12 month period. The contents of total lipids, neutral lipids, polar lipids and phospholipids were measured. The composition of phospholipids was determined by high‐performance liquid chromatography, and their fatty acid composition was analysed by gas chromatography. The phospholipid content ranged from 3.6 to 6.4 g kg^?1 soft tissue. PE (phosphatidyl ethanolamine) and PC (phosphatidyl choline) were the major constituents. C16:0, C20:5 and C22:6 were the major fatty acids. C20:5 (5.25–23.10%) and C22:6 (6.05–20.42%) varied regularly with the seasonal factors. Their total amounts were high from January to June, which would be an optimal time for the utilisation of the phospholipids of mussels. © 2002 Society of Chemical Industry