松材线虫病感病松树中致萎毒性物质的研究

本研究用我国自然感染松材线虫病的 15年生以上黑松和马尾松以及人工感染松材线虫病的 3年生黑松的木质组织进行萃取和粗提纯 ,方法为高压蒸煮法和氯仿碱法。生物测定结果显示 ,有致萎活性的毒性物质仅存在于自然感病未死的黑松和马尾松以及人工感病未死的黑松木质组织中。自然感病死后 1年的黑松和马尾松以及健康松树中不含有这些毒性物质。通过气相色谱—质谱联用仪 (GC MSSystem)对上述木质组织萃取物作定性分析发现 ,自然感病未死的黑松、马尾松和人工感病未死的黑松有致萎活性的萃取物中均含苯乙酸和 2 甲氧基肉桂酸 ,自然感病死后 1年的松树和健康松树中则无。而在健康松树和感病松树中都发现有苯甲醛存在。表明毒性物质与苯乙酸和 2 甲氧基肉桂酸有关 ,苯甲醛则是松树正常的代谢产物。苯乙酸和 2 甲氧基肉桂酸均为酚类化合物 ,是植物体内重要的次生物质。说明感病松树中的毒性物质是松树组织由于松材线虫侵染而产生的异常代谢产物 ,应称之为致萎毒性物质。

Diethylstilbestrol in Fish Tissue Determined Through Subcritical Fluid Extraction and with GC-MS

As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg^(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.

Determination of brominated diphenyl ethers in atmospheric particulate matter using selective pressurized liquid extraction and gas chromatography–mass spectrometry with a negative chemical ionization

This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.

Evaluation of Pesticide Residues in Mango by a Multi-residue Analysis and GC/MS Triple Quadrupole

Mango fruit has a great national and international market, and Brazilian production is 1,900 thousand tons/year exporting to North America and Europe. However, the loss could occur during the production when it is affected by pests and climate conditions, so the increased use of chemical substances and their presence should be monitored. A task for governmental agencies, producers and food sales, attending the sanitary barriers requirements, is to distribute food free from contaminants, so laboratories involved in this type of work usually employ multi-residues analysis. The objective of this study was to evaluate the presence of pesticide residues in mango using QuEChERS method and mass spectrometry technique. Positive samples were compared with Brazilian maximum residues level （MRL） and the health risk exposure was evaluated using the acute dietary intake （ADI） parameter. A total of 20 samples were collected from January to March, in Sao Paulo city markets. The recoveries were in the range of 70% to 120%, and standard deviation was below 20%. The category of pesticides not permitted for the crop were found in l0 samples; eight samples presented pesticides below MRL and two samples above MRL for the fungicide procloraz. The ADI values were below 20% of ADI for an adult and the worst case was dimethoate with 69% of ADI for children. The time spent in monitoring studies and the viability of method chosen must be considered by pesticide residues laboratories during routine analysis of food quality control.

Lipid Oxidation and Fatty Acid Composition in Salt-Dried Yellow Croaker(Pseudosciaena polyactis) During Processing

Lipid oxidation in salt-dried yellow croaker(Pseudosciaena polyactis) was evaluated during processing with commonly used analytical indices, such as the peroxide value(POV), the thiobarbituric acid reactive substances(TBARS) value, and oxidative-relative lipoxygenase(LOX) activity. Additionally, fatty acids were analyzed using gas chromatography-mass spectrometry. Both POV and TBARS increased significantly(P < 0.05) at the rinsing stage. POV reached its peak value of 3.63 meq O_2 per kg sample at the drying stage, whereas TBARS constantly increased from 0.05 to 0.20 mg MDA per kg sample. Processing of salt-dried yellow croaker had an extremely significant(P < 0.01) effect on LOX activity. Twenty-six fatty acids were identified. Combined eicosapentaenoic acid(EPA; C20:5n3) and docosahexaenoic acid(DHA; C22:6n3) content varied between(19.20 ±0.37) mg g^(-1) and(23.45 ± 1.05) mg g^(-1). The polyunsaturated fatty acid/saturated fatty acid(PUFA/SFA) ratio in yellow croaker was 0.73–1.10, and the n-6/n-3 PUFA ratio was approximately 0.13–0.20. The contents of most fatty acids varied significantly(P <0.05) during the different processing stages, and these differences were caused by lipid oxidation. C18:0, C16:1n7, C19:0, and C22:6n3 showed clear changes in principle component one of a principle components analysis. These fatty acids are potential markers for evaluating lipid oxidation in fish muscle because there was a significant correlation between these markers and TBARS and LOX activity(P < 0.05) with Pearson's coefficients > 0.931.

Economic and Qualitative Traits of Italian Alps Saffron

Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain multifunctional farms, with a positive impact on economy and land management. According to ISO 3632(2010/2011), saffron can be classified into three categories of quality(I, II, III) depending on the concentration of the three main metabolites responsible for its characteristic colour, flavor and aroma: Crocin, Picrocrocin and Safranal. This study represents the first investigation of the quality of saffron produced in the Italian Alps evaluated with spectrophotometry, HPLC, solid-phase microextraction(SPME), and gas chromatographic analysis combined with mass spectrometry(GC/MS). The experiments used Crocus sativus stigmas produced in 2012-2013 in different areas of the Central Italian Alps were located at an altitude between 720 and 1200 m a.s.l.. Results obtained were compared to commercial saffron. The analyses confirmed that all samples can be classified in the first quality category according to the ISO classification. This high quality is also confirmed by HPLC analysis. Moreover, the SPME-GC/MS analysis identified some differences in the aromatic profile of saffron samples, in particular regarding safranal concentration. A preliminary assessment of the economic viability of high quality saffron production for local markets was also performed. Our study provides valid information regarding the quality and economic sustainability of saffron production in the alpine area confirming this crop as a good candidate for a new source of income for multifunctional farms in mountain areas.