棉籽壳中除草活性物质提取及鉴定

为了开发利用棉籽壳中的除草活性物质，分别以无水乙醇、正丁醇、石油醚和乙酸乙酯为溶剂，采用索氏提取法对棉籽壳中的活性物质进行了提取，并对各溶剂粗提物进行了除草活性测定。结果发现:用无水乙醇提取的粗提物对稗草生长的抑制活性最高，经气相色谱-质谱(GC-MS)联用分析，发现该粗提物中主要含有甘油、三环己基3-烯-6-辛酮、4-乙烯基-2-甲氧基苯酚、(邻甲基苯酚)-2-溴-2氯-乙酰酯、十四酸、十四酸乙酯、十六烷酸、辛酸异戊酯和亚油酸9种化合物。进一步的除草活性测定结果表明，亚油酸、辛酸异戊酯、4-乙烯基-2-甲氧基苯酚和(邻甲基苯酚)-2-溴-2氯-乙酰酯4种化合物对稗草表现出一定的除草活性，其中亚油酸活性最强，其IC₅₀值为14.5 mg/L。     

超高效液相色谱—串联质谱法检测鸡血液样品中喹诺酮类药物残留

旨在建立鸡血液样品中多种喹诺酮类药物残留的超高效液相色谱—串联质谱方法。样品经乙腈提取,经Waters Acquity UPLC BEH C₁₈色谱柱分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子（ESI⁺）模式电离,MRM扫描模式检测。经方法学验证,该方法的线性关系、回收率、精密度均符合要求。应用超高效液相色谱—串联质谱法建立了鸡血液样品中多种喹诺酮类药物同时检测的方法,实现了动物血液样品中12种喹诺酮类药物同时定性、定量分析。     

氟吡菌胺及其代谢物在黄瓜中的残留

为评价氟吡菌胺及其代谢物在黄瓜上的安全性，建立了同时检测氟吡菌胺及其代谢物2，6-二氯苯甲酰胺的高效液相色谱-串联质谱法。前处理采用以乙腈提取，无水硫酸镁、石墨化碳（GCB）和乙二胺-N-丙基硅烷（PSA）为分散净化剂的QuEChERS方法，应用高效液相色谱-串联质谱仪在多反应监测（MRM）模式下进行检测。结果表明，在0.05~5 mg·kg^-1的加标范围内，氟吡菌胺和2，6-二氯苯甲酰胺的平均回收率分别为82%~98%和90%~100%，相对标准偏差（RSD，n=5）分别为1.6%~7.9%和3.2%~9.4%，定量检出限（LOQ）为0.05 mg·kg^-1。最终残留试验表明：在氟吡菌胺推荐剂量（735 g·hm^-2）下，施药3次，距最后一次施药间隔1、3 d和5 d时采收，氟吡菌胺及2，6-二氯苯甲酰胺在黄瓜上的最高残留量均小于0.05 mg·kg^-1，低于我国规定的氟吡菌胺在黄瓜中的最大残留限量0.5 mg·kg^-1。该方法前处理过程简单、方便、快速，灵敏度、准确度和精密度均满足残留分析的要求，可用于氟吡菌胺及代谢物2，6-二氯苯甲酰胺在黄瓜中的残留检测。     

广西西北喀斯特不同植被不同土层的土壤颗粒有机质

以广西西北喀斯特地区不同植被(草丛、灌丛、原生林)生态系统表层(0～10 cm)及深层(70～100 cm)土壤为研究对象,采用热裂解–气相–质谱(Pyr–TMAH–GC/MS)技术,研究不同植被表层与深层土壤颗粒有机质(POM)的变化特征。结果表明:表层土壤的pH值、有机碳、总氮、总磷、碱解氮、速效磷和速效钾含量均随植被的正向演替呈上升趋势;草丛表层土壤的有机碳、总磷和碱解氮含量均显著高于深层土壤的(P0.05);灌丛表层土壤的有机碳、总氮、总磷、碱解氮、速效磷和速效钾含量均显著高于深层土壤的(P0.05),灌丛表层土壤的pH值和总钾含量显著低于深层土壤的(P0.05);原生林表层土壤的总磷、速效磷和速效钾含量显著高于深层土壤的(P0.05);随着植被的正向演替,土壤POM总量呈增加趋势,表层土壤POM总量显著高于深层土壤的;土壤POM热裂解产物类型主要有木质素类、酚类、芳烃、多环芳烃及脂类化合物,木质素类化合物仅存在于表层土壤,稠环芳烃(此处指除萘和茚外的多环芳烃)占比则随植被的正向演替呈下降趋势;植被显著影响POM总量和POM热裂解产物中对羟基苯基、稠环芳烃、脂肪酸、正构烯烃、萘、氰的占比,土层深度显著影响POM总量和POM热裂解产物中对羟基苯基、愈创木基、丁香酚基、茚、脂肪酸、酮、苯、烷基苯、酚类和氰的占比,植被与土层的交互作用显著影响POM热裂解产物中对羟基苯基、萜烯和脂肪酸的占比;POM总量与有机碳、总氮、总磷、碱解氮、速效钾和速效磷含量呈显著正相关,与容重和总钾含量呈显著负相关,稠环芳烃与有机碳、总氮、总磷、碱解氮、速效磷和速效钾含量呈显著负相关,且碱解氮和pH值显著影响POM化合物组成。可见,在喀斯特地区,土壤POM含量能反映土壤中潜在活性养分含量,可作为喀斯特地区评价不同植被恢复对土壤有机质库及土壤质量动态变化影响的敏感指标。     

QuEChERS-超高效液相色谱-串联质谱技术同时测定大蒜中10种农药残留

建立了快速、准确测定大蒜中10种农药多残留的QuEChERS-超高效液相色谱-串联质谱检测技术。样品经酸化乙腈提取,无水硫酸镁(500 mg)除水后,用N-丙基乙二胺(PSA,500 mg)和十八烷基键合硅胶(C₁₈,500 mg)净化,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,Waters C₁₈色谱柱分离,采用正离子多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量。10种农药的检出限在0.020~0.800 μg·kg^-1,定量限在0.067~2.670 μg·kg^-1。线性范围内相关系数均大于0.99。加标回收率在73.4%~109.0%,相对标准偏差在1.2%~9.8%。结果表明,该方法简便、快速、灵敏度高、重现性好,可同时测定大蒜中10种农药。     

电感耦合等离子体质谱法测定农产品中的锗

采用微波消解处理农产品样品,电感耦合等离子体质谱法测定Ge,简单快速,检出限低。选用103Rh为内标,采用校正方程消除质谱干扰,经国家一级标准物质验证,方法准确度和精密度均满足实际样品分析的要求,回收率达到90%～110%。     

A systematic approach to determine the impact of elevated CO2 levels on the chemical composition of wheat (Triticum aestivum)

Two wheat genetic lines (responsive and non-responsive to elevated CO₂) grown under ambient and free-air CO₂ enrichment (FACE) conditions were compared using fuzzy chromatography mass spectrometry (FCMS) metabolite fingerprinting. A more comprehensive survey of the changes in their chemical composition was made on selected samples using ultra-high-performance liquid chromatography (UHPLC) metabolomic profiling with high resolution accurate mass/tandem mass spectrometry (HRAM/MSⁿ). Principal component analysis (PCA) of the metabolite fingerprints showed four clusters for the two genetic lines (responsive and non-responsive) and the two CO₂ levels (ambient and elevated) in score plots. Metabolite profiling of representative samples for each of the four clusters identified 25 and 16 compounds from negative and positive data, respectively, including amino acids, saccharides, phenolic acids, flavonoids, and lipids. Loading plots demonstrated that some saccharides and lipids were responsible for discriminating between not only two genetic lines but also two CO₂ levels. Analysis of free amino acids (not bound) showed a clear pattern of reduced concentration for both lines with elevated CO₂. After acid hydrolysis, the responsive line 6 (41% increase in yield) showed the same pattern observed for free amino acids, but the non-responsive line 5 (6% increase in yield) showed different trends in concentrations of amino acids with elevated CO₂.     

Localization of amino acids in germinated rice grain: Gamma-aminobutyric acid and essential amino acids production approach

Germinated rice is popularly consumed for its high gamma-aminobutyric acid (GABA) and bioactive compounds. Supporting information on how to germinate rice with high GABA content and essential amino acids is lacking. White and colored rough rice were germinated for 0, 24, 48, 72, 96, 120 and 144 h. GABA, GABA substrates and essential amino acids were also investigated using GC-MS and MALDI-MSI. GABA was more concentrated after germination and shifted into the coleoptile. High correlation was recorded between germination time and GABA (0.79–0.83, p ≤ 0.01) and glutamic acid (0.88–0.89, p ≤ 0.01). Highest rates of GABA and glutamic production were observed within 48 h of germination in both rice varieties (26.12 and 34.28 mg/100g) and reached maximum value at 96 h (31.36 and 38.75 mg/100g). Colored rice germination showed higher GABA, GABA substrates and deficient amino acids than white rice. GABA and essential amino acids drastically increased after germination, supporting the consumption of germinated rice as a functional food.     

Effects of germination and kilning on the phenolic compounds and nutritional properties of quinoa (Chenopodium quinoa) and kiwicha (Amaranthus caudatus)

Quinoa (Chenopodium quinoa) and kiwicha (Amaranthus caudatus) are nutritious pseudocereals that originate from the Andean region. The aim of this research was to study the effect of germination and the subsequent kilning on the phenolic compounds and proximate composition in selected Peruvian varieties of quinoa (“Chullpi”) and kiwicha (“Oscar Blanco”). The germination process was carried out for 24, 48 and 72 h at 22 °C, and the kilning was performed with samples germinated for 72 h by drying the seeds at 90 °C for 5 min. Both processes increased the protein content of the samples. However, lipid content was reduced during germination. On the other hand, germination and kilning clearly increased the concentration of total phenolic compounds in both quinoa and kiwicha. Germination for 72 h either with or without kilning process resulted in a significant (p < 0.05) increase in the total content of phenolics compared to untreated materials, which was especially due to coumaric acid and a kaempferol tri-glycoside in quinoa and caffeoylquinic acid in kiwicha. Based on the results, germination and kilning may improve the nutritional quality of the Andean grains, encouraging the usage of the processed grains as ingredients in functional products for people with special gluten-free or vegetarian diets.     

Recent progress in analytical method development to ensure the safety of gluten-free foods for celiac disease patients

As laid down by the Codex Alimentarius, products bearing a gluten-free label must not contain gluten levels above 20 mg/kg to be safe for consumption by celiac disease patients. Analytical methods to detect gluten from wheat, rye and barley need to be sufficiently sensitive, specific, suitable for routine analyses and validated by collaborative studies. With continuous progress in the field of gluten analysis, the aim of this paper is to provide an up-to-date overview of legislation regarding gluten-free products worldwide, as well as immunochemical, proteomics-based, genomics-based and other methods designed to analyse gluten traces. While ELISA test kits and PCR are still most widely used in quality control, liquid chromatography tandem mass spectrometry (LC-MS/MS) is gaining more and more importance by providing unprecedented insights into gluten. Several other methods such as immunosensors, other sensors and microarrays are being developed. The pro's and con's of the different methods are discussed as well as the remaining challenges, including the need for improved extraction procedures, comprehensive reference materials and independent reference methods.