西瓜中4种植物生长调节剂残留的分析方法研究

建立了固相萃取/高效液相色谱法测定西瓜中24-二氯苯氧乙酸(24-D)、赤霉素(GA3)、多效唑(PP333)、6-苄氨基嘌呤(6-BA) 4种植物生长调节剂残留的方法.样品用80%甲醇溶液提取,采用Strata C18固相萃取小柱进行富集、净化,以甲醇-0.15%磷酸水溶液为流动相,梯度洗脱,经ZORBAX Ec...     

离子液体添加剂[BMIM]HSO4对锌电积过程析氧反应动力学的影响

研究了1-丁基-3-甲基咪唑硫酸氢盐([BMIM]HSO₄)离子液体对锌电积过程析氧反应的影响. 研究工作借助于动电位极化, 电化学阻抗谱, 扫描电镜和X射线衍射等测试技术. 动电位极化曲线及对应的动力学参数分析表明, [BMIM]HSO₄对阳极析氧反应具有催化作用,可提高析氧反应速率常数. 电化学阻抗谱数据表明,[BMIM]HSO₄能显著降低阳极析氧电荷传递电阻,在所研究的1.85-2.10 V电位范围内添加5 mg·L^-1 [BMIM]HSO₄, 电阻值至少降低50%. 此外, 添加剂对阳极表面二次反应具有抑制作用, 其在阳极表面的吸附,阻碍了阴离子的阳极活化位点吸附过程. 电化学测试结果与长时间(120 h)阳极极化后所得阳极表面形貌和结晶取向分析结果相一致. [BMIM]HSO₄的添加能有效抑制中间产物β-PbO₂的形成,促进铅银电极表面大块且疏松多孔α-PbO₂的生成,加速阳极析氧的进行.     

液相色谱-串联质谱法检测动物源性食品中激素残留所遇到问题的探讨

探讨了液相色谱-串联质谱法用于动物源性食品中激素残留检测时关于样品的提取与净化、酶解、基质效应和激素来源等问题(引用文献29篇)。     

链接基团对固载手性Salen Mn(m)催化不对称环氧化反应的影响

制备了二胺和二酚修饰的晶态有机聚合物-无机杂化载体低聚苯乙烯基膦酸-膦酸氢锆(LCZSPP)轴向固载手性Salen Mn(Ⅲ)催化剂,将其应用于非官能烯烃的多相不对称环氧化反应.研究了两类轴向连接基团及助催化剂在催化不对称环氧化反应中的影响.结果表明,通过二胺为链接基团固载的催化剂在加入轴向助剂(NMO)的情况下,转化...     

应用超高效液相色谱-四极杆-飞行时间质谱建立茶叶中农药残留的筛查与确证方法

基于超高效液相色谱-四极杆-飞行时间质谱(UPLC-QTOF-MS),使用UNIFI软件建立91种农药残留的筛查与确证方法,进行定性方法验证并应用于流通市场中茶叶的筛查检测。通过对收集的农药认证标准物质(CRM)分析,构建91种农药化合物的质谱数据库。样品经乙腈提取,固相萃取柱净化,Acquity BEH C18色谱柱分离,在MS^E模式下进行全信息采集(ESI+), UNIFI软件对数据进行匹配分析。设置保留时间最大偏差为±0.1 min,精确质量偏差阈值为±5×10^-6,可识别加合物形式包括[M+H]⁺、[M+Na]⁺、[M+K]⁺、[M+NH₄]⁺。参照SANTE/11813/2017指南进行定性方法学验证。在21份茶叶样品中添加混合标准溶液至4个水平(0.01、0.05、0.10、0.20 mg/kg),确定每种农药在茶叶样品中的筛查检出限(SDL),共评估了1911种农药/样品组合。发现有66种农药的SDL为0.01 mg/kg, 8种农药的SDL为0.05 mg/kg, 1种农药的SDL为0.10 mg/kg, 3种农药的SDL为0.20 mg/kg,共有13种农药的SDL大于0.20 mg/kg。一种农药在筛查检测中存在基质抑制效应。最后,应用建立的方法分析了流通市场中22份茶叶样品的农药残留情况,从6份茶叶样品中筛查检测出6种农药化合物,经人工鉴定均为阳性。该法为茶叶中农药残留的高通量筛查检测提供了参考。     

Reliable screening of pesticide residues in maternal and umbilical cord sera by gas chromatography-quadrupole time of flight mass spectrometry

The widespread use of pesticides induces heavy adverse effects on human health,especially for the pregnant women and the newborns.In this study,a screening method has been developed for the determination of multi-pesticides in maternal and umbilical cord sera.All pesticides in sera were collected using solid phase extraction(SPE),and analyzed by gas chromatography-quadrupole time of flight mass spectrometry(GC-QTOF MS).To set up the quality criteria,a database of 50 pesticides was created and the accurate masses of 3 up to 5 representative ions with their intensity ratios were included for each pesticide.In addition,a novel"identification points"(IPs)system relying on the accurate MS1 and MS2 spectra was used to interpret the data for each suspected pesticide.The methodology was then applied to a pair of maternal and umbilical cord sera.A total of six pesticide residues were screened out successfully.In conclusion,GC-QTOF MS combined with an accurate mass database seemed to be one of the most efficient tools for systematic pesticide analysis.     

Multiresidue method for the fast determination of pesticides in nutraceutical products (Camellia sinensis) by GC coupled to triple quadrupole MS

A method based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) has been developed and validated for the determination and quantification of more than 140 pesticides in nutraceutical products obtained from green tea (Camellia sinensis). Extraction was performed with acidified acetonitrile (acetic acid 1%, v/v) and a clean‐up step using primary secondary amine (50 mg), graphitized black carbon (100 mg) and magnesium sulfate (200 mg) was needed. Pesticide determination was achieved utilizing GC coupled to triple quadrupole MS/MS using the selective‐reaction monitoring mode. The total run time was 23 min. Pesticides were quantified using matrix‐matched calibration. Recoveries ranged from 70 to 120% and relative SD was lower than 25% at 10, 50, and 100 μg/kg. LOQs were lower than 10 μg/kg. 148 pesticides were validated. The validated method was applied to commercial nutraceutical products, detecting 4,4‐dichlorobenzophenone (28 μg/kg), o,p′‐dicofol (38 μg/kg) and p,p‐dicofol (44 μg/kg) in a few samples.     

Simultaneous determination of ten organophosphate pesticide residues in fruits by gas chromatography coupled with magnetic separation

In this study, γ‐Fe₂O₃/chitosan magnetic microspheres were synthesized and evaluated by X‐ray diffraction, SEM, thermogravimetric analysis, and static and kinetic adsorption experiments. Results showed that the magnetic microspheres exhibited good adsorption ability, and offered fast kinetics for the adsorption of trichlorfon, methamidophos, malathion, methyl parathion, dimethoate, omethoate, phosphamidon, phorate, isocarbophos, and chlorpyrifos. Based on magnetic separation, a simple method of magnetic SPE coupled to GC for the simultaneous determination of ten trace organophosphate pesticide residues was developed. Under the optimal conditions, the enrichment factor for ten organophosphorus pesticides was 10.1–364.7 and linear range was 0.001–10.0 mg/L. The LOD (S/N = 3) of the method for the ten pesticides was 0.31–3.59 μg/kg. The RSD for three replicate extractions of spiked samples was between 2.5 and 6.3%. The pear and apple samples spiked with ten organophosphate pesticides at 20 and 200 μg/kg levels were extracted and determined by this method with good recoveries ranging from 79.9 to 98.7%. Moreover, the method has been successfully applied for the determination of the ten organophosphate pesticide residues in peach samples.     

Ambient ionisation mass spectrometry for the characterisation of polymers and polymer additives: A review

The purpose of this review is to showcase the present capabilities of ambient sampling and ionisation technologies for the analysis of polymers and polymer additives by mass spectrometry (MS) while simultaneously highlighting their advantages and limitations in a critical fashion. To qualify as an ambient ionisation technique, the method must be able to probe the surface of solid or liquid samples while operating in an open environment, allowing a variety of sample sizes, shapes, and substrate materials to be analysed. The main sections of this review will be guided by the underlying principle governing the desorption/extraction step of the analysis; liquid extraction, laser ablation, or thermal desorption, and the major component investigated, either the polymer itself or exogenous compounds (additives and contaminants) present within or on the polymer substrate. The review will conclude by summarising some of the challenges these technologies still face and possible directions that would further enhance the utility of ambient ionisation mass spectrometry as a tool for polymer analysis.     

基于拓扑优化和深度学习的新型结构生成方法

计算机辅助设计已广泛应用于结构计算和分析,但如何利用计算机智能生成最佳的新型结构还面临巨大挑战。针对这一问题,提出了一种基于拓扑优化和深度学习的新型结构智能生成方法。该方法首先通过结构拓扑优化分析获得不同参数下的优化结果制作训练集图片,并将训练集标签定义为相应的工况类型,然后应用最小二乘生成对抗网络(LSGAN)深度学习算法进行训练并生成大量的新型结构,最后建立评价指标和评估体系对生成的模型进行评价比较,根据需求选择最佳结构设计方案。结合一个铸钢支座节点底板设计的工程案例,详细阐述了上述方法的应用过程,并借助三维重构技术和增材制造技术实现结构模型的一体化制造。研究结果表明,基于拓扑优化和深度学习的新型结构智能生成方法不仅可以自动生成新的结构,而且可以进一步优化结构的材料用量和力学性能。