贵州不同海拔鱼腥草代谢产物主要特征

对贵州不同海拔鱼腥草中绿原酸、芦丁、槲皮素、槲皮苷、金丝桃苷、山奈素、异鼠李素、槲皮素-3-O-β-D-葡萄糖苷以及挥发性化学成分行研究,通过HPLC 分析绿原酸和黄酮类化合物,挥发性化学成分利用顶空固相微萃取结合气- 质联用(HS-SPME-GC/MS)进行分析,总挥发油的含量用水蒸气蒸馏提取获得。结果表明：鱼腥中绿原酸和黄酮的含量分别在海拔1400～1500m 和500～600m有较高的含量;鱼腥草精油在海拔600～700m有较高的含量,甲基正壬酮含量随海拔的增加而变化在700～800m 有较高的含量;单萜(蒎烯)、倍半萜(石竹烯(Ⅱ))、脂肪酮(甲基正壬酮)、脂肪酸(羊油酸)和脂肪酸酯(2,6,10,14- 四甲基十五酸甲酯)的含量在不同的海拔有显著的差异。     

中温杀菌对乳化肠挥发性风味物质变化的影响

以乳化肠为研究对象,分析中温杀菌与低温、高温杀菌带来的风味物质的变化规律。利用固相微萃取-气相色谱-质谱联用仪,分别对80℃低温杀菌、95℃中温杀菌、105℃中温杀菌和121℃高温杀菌的乳化肠的挥发性风味成分进行定性和半定量的分析。结果表明:4种热杀菌的乳化肠分别鉴定出39、39、41、37种挥发性风味物质,不同的热杀菌方式会导致挥发性风味物质种类和含量发生变化;对中温乳化肠风味贡献较大的化合物有:己醛、壬醛、1-辛烯-3-醇、2-戊基呋喃和2-甲氧基-4-(2-丙烯基)-苯酚。     

固相萃取净化-气相色谱法检测人乳中 持久性有机氯农药

目的 建立母乳中有机氯农药六六六和滴滴涕的检测方法, 并对北京、兰州和杭州三个地区的蓄积水平现状进行分析。方法 母乳样品用乙腈提取, 经过酸化的硅胶固相萃取柱净化, 浓缩后, 采用气相色谱仪检测。结果 8种农药的线性范围在5~200 ng/mL, 相关系数0.9955~0.9994, 定量限均小于2.6 μg/kg, 平均回收率在70%~122%, 相对标准偏差在3.91%~10.77%。结论 本方法结合磺化法和固相萃取法, 能有效去除基质中的杂质。通过方法学验证证明, 本方法操作简单、精确、快速, 适用于母乳中有机氯的检测。随着六六六、滴滴涕等持久性有机氯农药的禁用或严格限用, 母乳中持久性有机氯农药的蓄积水平明显降低。     

基质固相分散-高效液相色谱法测定川味香肠中的苏丹红染料

建立了川味香肠中苏丹红I～IV的基质固相分散(MSPD)-高效液相色谱(HPLC)分析方法。样品以无水硫酸钠作为分散基体,研磨均匀后与中性氧化铝同时装柱,正己烷淋洗净化,以丙酮-正己烷(5∶95,V/V)溶液洗脱。用InertsilODS-spC18柱(4.6mm×250mm,5μm)进行分离,流动相A为含0.1%甲酸的甲醇,流动相B为0.02mol/L的乙酸铵溶液(A∶B=85∶15,V/V),等度洗脱,柱温40℃。二极管阵列检测器检测,检测波长为490nm,利用保留时间和光谱图定性,外标法定量。4种苏丹红染料在0.10～50.00μg/mL范围内线性关系良好,相关系数均大于0.9999,苏丹红I、II、III、IV的检出限(LOD)分别为0.008～0.011mg/kg(信噪比S/N=3)。在添加浓度为5.0～25.0mg/kg范围内平均回收率达85.54%～94.66%,相对标准偏差(RSD)为0.87%～4.23%(n=6)。     

Quantitative Analysis of Bioactive Compounds from Aromatic Plants by Means of Dynamic Headspace Extraction and Multiple Headspace Extraction‐Gas Chromatography‐Mass Spectrometry

Seven monoterpenes in 4 aromatic plants (sage, cardamom, lavender, and rosemary) were quantified in liquid extracts and directly in solid samples by means of dynamic headspace‐gas chromatography‐mass spectrometry (DHS‐GC‐MS) and multiple headspace extraction‐gas chromatography‐mass spectrometry (MHSE), respectively. The monoterpenes were 1st extracted by means of supercritical fluid extraction (SFE) and analyzed by an optimized DHS‐GC‐MS. The optimization of the dynamic extraction step and the desorption/cryo‐focusing step were tackled independently by experimental design assays. The best working conditions were set at 30 °C for the incubation temperature, 5 min of incubation time, and 40 mL of purge volume for the dynamic extraction step of these bioactive molecules. The conditions of the desorption/cryo‐trapping step from the Tenax TA trap were set at follows: the temperature was increased from 30 to 300 °C at 150 °C/min, although the cryo‐trapping was maintained at ?70 °C. In order to estimate the efficiency of the SFE process, the analysis of monoterpenes in the 4 aromatic plants was directly carried out by means of MHSE because it did not require any sample preparation. Good linearity (r² > 0.99) and reproducibility (relative standard deviation % <12) was obtained for solid and liquid quantification approaches, in the ranges of 0.5 to 200 ng and 10 to 500 ng/mL, respectively. The developed methods were applied to analyze the concentration of 7 monoterpenes in aromatic plants obtaining concentrations in the range of 2 to 6000 ng/g and 0.25 to 110 μg/mg, respectively.     

静态顶空气相色谱法测定黄酒中β-苯乙醇的含量

目的:建立一套静态顶空气相色谱法测定黄酒中β-苯乙醇含量的分析方法。方法:在顶空进样瓶中,β-苯乙醇在气液两相平衡分配后,取顶部空间气态样品进行气相色谱分析。结果:β-苯乙醇在20.20mg/L~161.63mg/L浓度范围内,线性相关系数r=0.9996,方法检出限为1mg/L,RSD为2.04%~3.42%,回收率在91.7%~98.4%之间。     

Determination of pesticide residues in food matrices using the QuEChERS methodology

The determination of pesticide residues in food matrices is a formidable challenge mainly because of the small quantities of analytes and large amounts of interfering substances which can be co-extracted with analytes and, in most cases, adversely affect the results of an analysis. However, safety concerns require that pesticides of the wide range of chemical properties (including acidic, basic and neutral) should be monitored. Because of the wide variety of food matrices, the sample must initially be cleaned up before final analysis. That is why the analytical chemist is faced with the need to devise new methodologies for determining such residues to be determined in a single analytical run. To accomplish the goal, QuEChERS methodology has been developed. It is a streamlined and effective extraction and cleanup approach for the analysis of diverse analyte residues in food matrices. So far, there have been achieved promising results by liquid or gas chromatography analysis, including pesticides, but also acrylamide, pharmaceuticals and veterinary drugs.     

顶空气相色谱用于聚丙烯腈溶液中残留丙烯腈的检测

介绍了一种测定浆丙烯腈溶液中丙烯腈单体的方法,同时对聚合物含量、平衡时间、平衡温度及顶空体积对测定结果的影响进行了分析。将已稀释的溶液移入顶窄瓶中,在设定温度下达到气液平衡后进入气相色谱仪中测定。该法的检出限达2．5ppm,线性相关系数为0．9979,相对标准偏差小于5％,阐收率为96．1％-103．9％。     

机械合金化合成YAlO3

为了合成YAlO3(YAP),对Y2O3-Al2O3粉体混合物进行了高能球磨研究。试验结果表明:经高能球磨后,Y2O3-Al2O3可发生固相合成反应,生成YAlO3。Y2O3-Al2O3的机械合金化过程包括两个阶段:第一阶段(0～2h),氧化物颗粒快速细化,晶格发生严重畸变,球磨促使Y2O3发生了晶型转变,由稳定的立方晶转变成非稳态的单斜晶;第二阶段(5～40h),Y2O3晶型转变完成,并呈无定形化,Y2O3和Al2O3发生固相合成反应,生成YAlO3。     

超高压处理对桃汁挥发性化学成分的影响

利用超高压装置(400 MPa,25℃,20 min)处理桃汁,采用顶空固相微萃取与毛细管气相色谱-质谱联用技术检测桃汁中的挥发性成分,并用面积归一化法测定了各种成分的相对质量分数。经与超高压处理前桃子原汁的41种主要香气成分分析比较发现,超高压处理后桃汁中主要特征香气成分的质量分数明显增加,其中γ-己内酯、cis-2-己烯醇、γ-癸内酯、叶醇和己醇等物质的质量分数分别增长了41.7%、52.0%、109.5%、288%、313.1%,并且新增加了乙酸己酯(0.29%)、cis-2-己烯醇乙酸酯(0.13%)、cis-3-己烯醇乙酸酯(0.47%)和十八醛(0.41%)等香气成分;感官评定表明,桃汁的青鲜香气更加突出,说明超高压处理增强了桃汁的特征香气。