QuEChERS/气相色谱三重四级杆质谱法测定枸杞籽油中多环芳烃类物质

建立了同时检测保健食品枸杞籽油中16种多环芳烃(PAHs)的QuEChERS/气相色谱三重四级杆质谱(GC-MS/MS)方法。样品(0. 5 g)经3 mL乙腈提取2次,采用含200 mg PSA和100 mg C18吸附填料粉进行净化,净化后采用GC-MS/MS进行分析测定。结果表明:在优化条件下,16种PAHs分离度良好,在1. 0～200 ng/mL范围内线性关系良好;回收率为60. 04%～119. 00%,RSD在2. 92%～13. 03%之间;检出限在0. 2～3. 5μg/kg之间,定量限在0. 7～11. 5μg/kg之间。该方法数据可靠、简便快速、灵敏度高,适合保健食品枸杞籽油中多环芳烃的测定。     

鲟鱼传统发酵过程中挥发性风味物质的分析评价

以鲟鱼为原料,采用固相微萃取-气相色谱-质谱联用法,研究其发酵过程中挥发性风味物质种类和相对含量的变化情况,结合感觉阈值,采用相对气味活度值评价挥发性风味物质对总体风味的影响,探讨发酵过程中的关键性风味物质。分别检测新鲜鲟鱼,腌制鲟鱼,发酵5、10、20、25、35 d 7个阶段的挥发性风味物质,结果表明:新鲜、腌制、发酵5、10、20、25、35 d 7个阶段的挥发性风味物质种类分别为38、48、66、72、75、76种和84种。新鲜鲟鱼肉的主体风味物质为2,4-癸二烯醛、1-辛烯-3-醇、壬醛、癸醛、己醛等;腌制后的鲟鱼肉主体风味物质为壬醛、1-辛烯-3-醇、己醛、癸醛、柠檬烯等;发酵5 d鲟鱼肉的主体风味物质为1-辛烯-3-醇、柠檬烯、壬醛、乙酸乙酯、庚醇等;发酵10 d鲟鱼肉的主体风味物质为壬醛、1-辛烯-3-醇、乙酸乙酯、柠檬烯、癸醛等;发酵20 d鲟鱼肉的主体风味物质为壬醛、柠檬烯、1-辛烯-3-醇、癸醛、乙酸乙酯等;发酵25 d鲟鱼肉的主体风味物质为壬醛、柠檬烯、1-辛烯-3-醇、乙酸乙酯、癸醛等;发酵35 d鲟鱼肉的主体风味物质为乙酸乙酯、柠檬烯、壬醛、1-辛烯-3-醇、庚醇等。     

兼香型年份酒中香味物质的分析

通过单因素试验优化顶空固相微萃取（HS-SPME）条件，并结合气相色谱-质谱（GC-MS）技术研究兼香型年份酒中香味物质成分含量及差异。结果表明，最佳HS-SPME萃取条件为酒样酒精度14%vol，萃取温度40 ℃，萃取时间30 min，解吸时间5 min。GC-MS法共鉴定出67种挥发性风味物质，包括50种酯类，3种醇类，5种酸类，1种芳香族化合物，1种含硫化合物，2种呋喃类，3种酮类和2种醛类。酯类、醇类、酸类和呋喃类总含量随贮藏年份增长呈现上升趋势，醛类和酮类总含量变化规律不明显。经香气活度值（OAV）分析，确定出22种（OAV＞1）成分对白酒香味有贡献，其中有9种（OAV＞10）为重要香气成分，酯类为白酒香气的主要贡献物质。     

QuEChERS结合GC-MS/MS法测定果蔬汁中21种农药残留

建立一种采用QuEChERS前处理结合Quick Pro净化柱-气相色谱串联质谱（GC-MS/MS）法测定果蔬汁中的21种农药残留量的方法。样品采用乙腈提取，EN方法盐包盐析，经Quick Pro净化柱净化，DB-35MS UI色谱柱分离，采用选择离子监测（SIM）模式扫描，外标法定量。在质量浓度0.01～0.50 μg/mL范围内相关系数（R）均＞0.995，样品在0.01 mg/kg、0.02 mg/kg、0.10 mg/kg的添加水平下，21种农药的回收率在75.2%～117.8%之间，回收率实验结果相对标准偏差（RSD）在1.9%～11.5%之间。该方法操作简便，分析时间短，精密度好，适用于果蔬汁中多种农药残留的检测。     

梅花鹿鹿油的提取及成分检测

采用超临界CO2提取法从梅花鹿(Cervus nippon)鹿脂肪中提取鹿油,探讨提取工艺对鹿油提取率的影响。以鹿脂肪为原料,通过单因素试验和正交试验分别研究提取温度、提取压力、提取时间以及CO2流量对鹿油提取率的影响。研究结果表明,最佳的提取工艺为:提取温度45℃、提取压力40 MPa、提取时间150 min、CO2流量14 L/h。此时鹿油的提取率为44.81%。通过气相色谱-质谱法(gas chromatography mass spectrometry,GC-MS)联用对鹿油的成分进行检测,确定其含有16种脂肪酸,其中饱和脂肪酸和不饱和脂肪酸相对含量分别为69.840 9%和30.159 1%,主要脂肪酸有十六烷酸、十八烷酸及十八碳烯酸。     

Thermal degradation of corn starch based biodegradable plastic plates and determination of kinetic parameters by isoconversional methods using thermogravimetric analyzer

Oil shortage and awareness of environment pollution leads to the extensive use of biodegradable starch-based materials against synthetic plastics. The accumulated wastes of these plastics takes more time for natural recycling and the process is complex. Therefore the best option of recycling would be to convert these polymers into a source of energy by pyrolysis. So to understand the pyrolytic behaviour, kinetics of such waste plastics is studied by using thermogravimetric analysis at different heating rates of 10 °C, 20 °C, 40 °C, 60 °C, 80 °C and 100 °C in nitrogen atmosphere followed by characterization of the pyrolysis products. The kinetic parameters are obtained for two major stages of decomposition in two different temperature ranges 250–620 °C and 620–855 °C by iso-conversional methods such as Friedman, Coats-Redfern, FWO and Kissinger methods. The regression coefficient data (>0.9) of kinetic plots obtained for different methods best fits to the kinetic equation. Empirical formula of the compound is determined by ultimate analysis is CH_2.214S_0.0018O_0.6910. Proximate analysis gives the idea of volatile component which is74.33%. The range of average value of activation energy is 120.7013 kJ/mol to 140.7707 kJ/mol for the biodegradable plastic plate with different conversion (0.1–0.6) and (0.1–0.3) respectively at two different temperatures. The pyrolysis products obtained using a semi-batch reactor are characterized to know their composition and other properties.     

Food safety traits of mussels and clams: distribution of PCBs,PBDEs, OCPs,PAHs and PFASs in sample from different areas using HRMS-Orbitrap® and modified QuEChERS extraction followed by GC-MS/MS

Reviewing the presence of contaminant residues is important both for food safety and for monitoring of environmental pollution. Here, the occurrence of 6 polychlorinated biphenyls (PCBs), 15 organochlorine pesticides (OCPs), 7 polybrominated diphenyl ethers (PBDEs), 4 polycyclic aromatic hydrocarbons (PAHs) and 17 perfluoroalkyl substances (PFASs) was evaluated in mussels and clams. A liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) and an innovative QuEChERS extraction followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) methods were developed, validated and applied. We demonstrate good linearity, repeatability and accuracy of these methods, confirming that they are suitable for the analyses of mollusc samples. The prevalence of PCBs, OCPs and PAHs was higher in mussels than in clams. For PFASs, contamination was higher in clams than in mussels. The samples were all compliant with the regulations, and, for the compounds without legislative limits, a risk assessment confirmed that the values were lower than the tolerable intakes.     

GC-MS分析使用不同提取工艺获得的沙枣花挥发性成分

这项研究采用水蒸气蒸馏法、有机溶剂浸提法、真空泵抽取吸附采集法、固相微萃取法以及超临界CO2萃取法对新疆沙枣花挥发油进行提取,并探讨不同提取方法对沙枣花挥发性化合物成分的影响。通过气相色谱-质谱(GC-MS)联用技术对沙枣花挥发油的化学成分进行分析鉴定,用峰面积归一法确定各组分的相对含量。共分离鉴定出139种化合物,其中共检测出烃类22种(占21.3%)、醛类10种(占1.38%)、酯类47种(占62.18%)、酮类7种(占0.6%)、醇类21种(占9.52%)、酸类14种(占1.86%)、苯环类7种(占1.66%)、酚类5种(占1.14%)、其它物质6种(占0.33%)。其中共有成分4种,分别是2,3-丁二醇、苯乙酸乙酯、苯乙醇、反式-肉桂酸乙酯。     

5种脱色剂对粗鱼油挥发性风味物质及脂肪酸组成的影响

为探究凹凸棒土、硅藻土、活性炭、沸石及活性白土5种脱色剂对粗鱼油挥发性风味物质及脂肪酸组成的影响,采用气相色谱仪和顶空固相微萃取-气相色谱-质谱联用仪,对脱色鱼油的挥发性风味物质及脂肪酸的相对含量进行测定分析,并结合感觉阈值确定该鱼油主体风味成分。结果表明,赋予鱼油腥味、脂肪香味、蜡香等主要风味的壬醛、己醛、2-壬酮,其相对含量经脱色后有明显降低,风味改善效果显著。脱色后,鱼油的饱和脂肪酸相对含量呈下降趋势,而不饱和脂肪酸的相对含量则有增加趋势;酸价与过氧化值变化差异较大,而碘值及皂化值则无明显变化。凹凸棒土和活性白土脱色效果最佳,但脱腥效果较硅藻土、活性炭和沸石差。本研究结果对改善鱼油脱色工艺及脱色剂选择和不良风味等方面有一定理论指导意义。     

Research on paraffin removal and prevention by Bacillus spp. in high-salinity reservoirs

Problems in paraffin deposition occur frequently in oil exploitation. Considering the problem that some paraffin removal and prevention strains cannot grow in high-salinity reservoirs, we domesticated four salt-tolerant laboratory bacterial strains. Crude oil emulsification effect, paraffin removal rate, and paraffin prevention rate of the strains were evaluated. KB and JH-A strains exhibited good paraffin removal and prevention effects, with paraffin removal rates of 51.82% and 81.56%; and 51.82% and 80.90%, respectively. Gas chromatography mass spectrometry analysis of paraffin components before and after biodegradation was performed on KB and JH-A strains. Results showed that relative contents of n-alkanes between C15–C23 and C27–C30 evidently decreased, indicating their good biodegradation. This technique provides a new method for practical application of paraffin removal and prevention in high-salinity reservoirs.