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。     

Disulphide structure of high-molecular-weight (HMW-) gliadins as affected by terminators

This study aimed at elucidating SS-bonds of HMW-gliadins (HGL) from wheat with the focus on terminators of glutenin polymerisation. HGL from wheat flour extracts non-treated or treated with the S-alkylation reagent N-ethylmaleinimide (NEMI) were compared. HGL from wheat flour Akteur were isolated, hydrolysed with thermolysin and the resulting peptides pre-separated by gel permeation chromatography and analysed by liquid chromatography/mass-spectrometry using alternating electron transfer dissociation/collision-induced dissociation. Altogether, 22 and 28 SS-peptides from samples without and with NEMI treatment, respectively, were identified. Twenty-six peptides included standard SS-bonds of α- and γ-gliadins, high-molecular-weight and low-molecular-weight glutenin subunits. Eleven SS-bonds were identified for the first time. Fifteen peptides unique to HGL contained cysteine residues from gliadins with an odd number of cysteines (ω5-, α- and γ-gliadins). Thus, gliadins with an odd number of cysteines, glutathione and cysteine had acted as terminators of glutenin polymerisation. Decisive differences between samples without and with NEMI treatment were not obvious showing that the termination of polymerisation was already completed in the flour. The two HGL samples, however, were different in the majority of ten peptides that included disulphide-linked low-molecular-weight (LMW) thiols such as glutathione and cysteine with the former being enriched in the non-treated HGL-sample.     

terraGIS – a web GIS for delivery of digital soil maps in cotton‐growing areas of Australia

Effective management of soil requires the spatial distribution of its various physical, chemical and hydrological properties. This is because properties, for example clay content, determine the ability of soil to hold cations and retain water. However, data acquisition is labour intensive and time‐consuming. To add value to the limited soil data, remote sensing (e.g. airborne gamma‐ray spectrometry) and proximal sensing, such as electromagnetic (EM) induction, are being used as ancillary data. Here, we provide examples of developing Digital Soil Maps (DSM) of soil physical, chemical and hydrological properties, for seven cotton‐growing areas of southeastern Australia, by coupling soil data with remote and proximal sensed ancillary data. A greater challenge is how to get these DSM to a stakeholder in a way that is useful for practical soil use and management. This study describes how we facilitate access to the DSMs, using a simple‐to‐use web GIS platform, called terraGIS. The platform is underpinned by Google Maps API, which is an open‐source development environment for building spatially enabled Internet applications. In conclusion, we consider that terraGIS and the supporting information, available on the sister web page ( http://www.terragis.bees.unsw.edu.au/ ), allow easy access to explanation of DSM of soil properties, which are relevant to cotton growers, farm managers, consultants, extension staff, researchers, state and federal government agency personnel and policy analysts. Future work should be aimed at developing error budget maps to identify where additional soil and/or ancillary data is required to improve the accuracy of the DSMs.     

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。     

香蕉中噻唑膦残留分析方法研究

建立香蕉中噻唑膦的超高效液相色谱串联质谱法(UPLC-MS/MS)残留测定方法。香蕉样品采用乙腈提取和PSA+C18分散固相萃取,采用UPLC-MS/MS多反应模式(MRM)进行分析测定。噻唑膦在添加水平0.01~1.0 mg/kg范围内,平均回收率为94.3%~107.5%,相对标准偏差为7.9%~11.0%。采用外标法定量,方法的检出限为0.001μg/m L,定量限为0.005 mg/kg。该方法简单、准确、重复性较好且节省溶剂,适用于香蕉中噻唑膦的残留检测。     

低温风干工艺下酱鸭加工过程中品质特性变化规律研究

为改善酱鸭的质地、色泽和风味,本试验在传统酱鸭加工工艺的基础上,引入低温风干工艺制备酱鸭,并研究其加工过程中理化特性(水分含量、色泽、剪切力值、质构特性)和挥发性风味成分的变化。结果表明,在加工过程中,酱鸭水分含量从76.55%降至58.27%(P0.05);与原料肉相比,L~*值在风干6 h显著降低,a~*值在腌制和风干结束下降,b~*值和咀嚼性在酱制阶段增加,杀菌阶段下降,硬度在酱制阶段升高,而弹性和内聚性均在杀菌阶段降低;与风干24 h相比,胶着性在杀菌阶段降低(P0.05),剪切力值先升高后下降。酱鸭挥发性风味成分分析显示,酱鸭成品有70种挥发性风味成分,主要为萜烯类、醛类、呋喃类、酮类、烃类和醇类;其中,莰烯、己醛和2-戊基呋喃是酱鸭成品主要的特征风味成分,分别占总相对含量的16.51%、10.44%和11.88%。本试验结果为低温风干工艺下酱鸭品质变化特征的研究提供了一定的理论依据。     

基于GC-MS顶空进样法鉴别瘿木降香黄檀与大果紫檀

分别对两个批次含瘿瘤的降香黄檀和大果紫檀木材,采用GC-MS技术顶空进样方式,获取其总离子流图并进行相关系数、系统聚类和特征性化学成分分析。结果表明:两种木材之间总离子流图差别大,无相关性,而同种木材不同批次间相似度高,均含有相同的特征峰,相关系数高(R>0.900);系统聚类分析进一步验证了该试验结果;两种含瘿瘤木材主要特征化学成分种类和含量也完全不同;相关性分析、聚类分析和特征性成分分析均可鉴别区分这两种含瘿瘤木材,解决了含瘿瘤木材传统方法难以鉴别的难题。     

超高效液相色谱串联质谱非衍生化法测定土壤中草甘膦及其代谢物氨甲基膦酸含量

为了建立土壤中草甘膦(Glyphosate）及其主要代谢物氨甲基膦酸(AMPA)残留的定量分析方法,采用固相萃取结合液相色谱串联质谱技术,样品以磷酸钠和柠檬酸三钠混合溶液提取,经固相萃取柱净化,采用正向亲水性液相色谱柱(Hilic)梯度洗脱,通过质谱的多反应监测(MRM)负离子模式扫描进行测定,外标法定量。结果表明:草甘膦、氨甲基膦酸的线性范围为0.02~0.2 μg/mL,相关系数(R²)分别为0.9995、0.9998,检出限分别为0.5 μg/kg和0.6 μg/kg,定量限分别为1.6 μg/kg和2.0 μg/kg;3个加标水平草甘膦的回收率在79.67%~96.17%之间,AMPA回收率在77.83%~99.47%之间,RSD值分别为3.95%~7.49%、1.96%~3.89%。与传统的柱前衍生方法相比,具有前处理简单、检出限低、灵敏度高的优点,完全可以适用于土壤中草甘膦的分析。     

基于气相离子迁移谱的热处理对催熟香蕉的挥发性物质分析

以香蕉果实为试验材料,利用热激、低温和催熟处理采后香蕉果实,采用气相离子迁移谱检测香蕉的挥发性物质,研究热处理对催熟香蕉果实挥发性物质的影响。结果表明:与对照相比,7 ℃ 6 d+催熟3 d和H+7 ℃ 6 d+催熟3 d 2个处理均明显降低了糠醇、苯甲醛、4-甲基苯酚、己酸乙酯、二甲基二氧杂环酮、1-戊醇、己二酮、3-甲基丁酸、2-甲氧基苯酚、2-己醇、丁酸乙酯等组分的含量;相反,这2个处理均明显增加了丙醇、乙酸丙酯、戊酮-2,3-二酮、二甲基二硫、2,3-丁二醇、甲基吡嗪、3-甲基丁酸乙酯、α-蒎烯、1-辛烯-3-醇、二甘醇二甲醚、E-2-辛烯醛、E,Z-2,6-壬醛、顺式-3-己烯醇、辛酸、庚烷-2-酮等组分的含量。另外,H+7 ℃ 6 d+催熟3 d处理明显增加了羟基丙酮、3-甲基-3-丁烯-1-醇、3-甲基-2-丁醇等组分的含量。与7 ℃ 6 d+催熟3 d相比,H+7 ℃ 6 d+催熟3 d处理明显降低了三乙胺、苯酚、2-戊酮、2-戊基呋喃、癸醛、E-2-辛烯醛、甲硫基丙醛、2-己醇、2,3,5-三甲基吡嗪等组分的含量,导致这些组分含量与对照基本一致。进一步研究发现,热处理能明显降低7 ℃冷藏香蕉果实的冷害指数,减轻香蕉果实的冷害症状。热处理诱导催熟香蕉果实上述挥发性物质的变化,可能与热处理诱导香蕉果实产生抗冷性的过程密切相关。     

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.