液相色谱-串联质谱法测定动物性食品中20种抗生素类药物残留

建立了一种专属、灵敏的方法用于同时检测动物性食品中β-内酰胺类青霉素类抗生素、大环内酯类抗生素、四环族抗生素和林可胺类共20 种抗生素药物残留.首先对动物性食品中的抗生素类药物进行提取,再经HLB固相萃取柱净化,采用电喷雾离子源,以正离子检测方式进行质谱分析.实验结果表明,在10-200 μg/L质量浓度范围内上述20...     

铝合金高温断裂韧性的研究

通过6063铝合金的标准试验,确定了常温和高温下材料的弹性模量、屈服强度、破坏强度和应力强度因子。分别采用双线性和理想弹塑性模型,在ABAQUS平台上对标准CT试样的断裂韧性测试过程进行了数值模拟,计算了J积分,得到的应力强度因子和试验值误差4%,模拟的失稳扩展现象与实验所观察的现象一致。     

Abnormal Visible Luminescence Mechanism of Tb^3＋-Yb^3＋ Codoped SiOu-Al2O3-CaF2 Glass Studied by Time-Resolved Spectra

The upconversion energy transfer mechanism in Tb^3＋-Yb^3＋ co-doped SiO2-Al2O3-CaF2 glass is investigated by time-resolved spectra. The effect of donor ion Yb^3＋ is involved in the dynamic decay behavior of acceptor ion Tb^3＋, which provides direct proof for the energy transfer from Yb^3＋ to Tb^3＋. The pump power dependence curves show that the upconversion luminescence is a two-photon process. The measured decay curves of the 5D4 state （Tb^3＋） contain two parts： a slow decay process corresponding to its radiation, and a fast one with a decay parameter approximately twice the lifetime of the ^2F5/2 state （Yb^3＋ ）. The fast decay process is contradictory to the generally accepted cooperative sensitization upconversion rate equation model. Since the effect of the host environmental is excluded by comparative experiments, we believe that there should be another energy transfer mechanism in Tb^3＋-Yb^3＋ co-doped SiO2-Al2O3-CaF2 glass in addition to the cooperative sensitization process.     

施用污泥堆肥对土壤和小白菜重金属积累的影响

以金华市污水处理厂污泥为研究对象,利用它对小白菜进行的盆栽试验,研究了以污泥作堆肥对土壤和小白菜重金属积累的影响.结果表明,随着污泥堆肥施用量的增加,土壤和小白菜地上部组织的Cu、Zn、Cd和Pb含量也呈积累趋势,当施用量为10%时,地上部组织的重金属含量超过国家食品卫生标准.由此说明,在污泥堆肥和利用过程中应进一步严格控制重金属及其在作物体中积累,尤其控制可食部分中重金属的含量和污泥堆肥长期施用过程中的重金属在土壤和作物中的积累.     

土壤中吡虫啉加速溶剂萃取和传统提取方法对比研究

对土壤样品中吡虫啉快速压力溶剂萃取技术(PSE)与传统提取方法(超声波萃取、振荡提取和索氏萃取)进行了对比研究。结合固相萃取柱(SPE)净化-HPLC测定技术比较了4种提取方法对土壤样品中吡虫啉的提取效果。探讨了温度对PSE的影响,确定在萃取压力100bar、温度80℃条件下,PSE效果最好,3个土壤样品不同添加浓度下,吡虫啉平均回收率均大于85%,标准偏差小于2.5%。与从土壤中提取吡虫啉的传统方法相比,PSE回收率高于超声波萃取和振荡提取,其重现性和回收率与索氏萃取相当甚至更好,而且PSE避免了使用超声波萃取和振荡提取所带来的多次清洗的问题,节省溶剂;比索氏萃取节省时间。     

复合免疫亲和柱净化-液相色谱-串联质谱法测定动物源食品中6种黄曲霉毒素和6种玉米赤霉醇类真菌毒素残留量

建立了动物源食品(猪肉、鱼肉、猪肝)中6种黄曲霉毒素(AFB1、AFB2、AFG1、AFG2、AFM1和 AFM2)和6种玉米赤霉醇类真菌毒素(α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮和玉米赤霉烯酮)残留量的复合免疫亲和柱净化-高效液相色谱-串联质谱(HPLC-MS/ MS)检测方法。样品经β-葡萄糖苷酸/硫酸酯复合酶酶解后,用甲醇-乙腈(20∶80, V/ V)提取,提取液经玻璃纤维滤纸过滤,滤液用PBS 溶液稀释,复合免疫亲和柱富集和净化后,采用 HPLC-MS/ MS 法分析。12种目标分析物中 AFB2和 AFG2的线性范围为0.03~6.0μg/ L,其余目标分析物的线性范围为0.05~20μg/ L,线性相关系数均大于0.999,检出限在0.01~0.03μg/ kg 范围内,定量限在0.04~0.09μg/ kg 范围内。分别以0.5,1.0和5.0μg/ kg 添加浓度水平进行方法学验证,平均回收率为73.6%~98.4%,相对标准偏差(RSD)为1.9%~11.2%。本方法简便、灵敏,能够满足动物源食品中痕量黄曲霉毒素和玉米赤霉醇类真菌毒素残留的测定要求。     

铝合金化学成分标准物质的研制

介绍铝合金化学成分标准物质的研制过程。采用中频感应电炉熔炼法制备了铝合金化学成分标准物质候选物,并对标准物质候选物的均匀性和稳定性进行了考察。选择6家具有资质的实验室对研制的标准物质中各化学成分进行协作定值,并对各元素定值的不确定度进行评定。结果表明,在95%的置信区间内标准物质均匀性良好,经过13个月稳定性考察试验,标准物质稳定性良好。Si,Fe,Cu,Mn,Mg,Ti,Cd,V,Zr,B,Sn,Zn的定值结果分别为0.013 8%,0.012 5%,2.868%,0.185%,0.014 0%,0.082 8%,0.041 7%,0.032 9%,0.031 4%,0.003 8%,0.003 4%,0.025 6%,定值结果的相对扩展不确定度为1.4%~9.0%(k=2)。研制的标准物质达到相关技术要求,可用于该类铝合金材料的质量控制。     

分子磁体与环境的纠缠和退相干

本文研究了双轴分子磁体在耗散环境中的相干量子隧穿,作为环境的声子库抑制了相干量子隧穿,从而引起分子磁体中薛定谔猫态的退相干. 而环境内部声子之间的相互作用会导致分子磁体与热库之间退耦合,于是对退相干有一定的抑制作用. 在绝热近似和非绝热近似下,借助于约化密度矩阵计算了超Ohmo耗散中分子磁体与环境之间的纠缠度,当纠缠达到最大时,相干隧穿被完全抑制.     

提升高三化学复习课效益的几点思考

高三化学复习课的效益堪忧,其成因来源于操作主体和操作形式两方面。提升复习课效益应解决思维容量、诊断方式和结构优化等问题。提升策略可从思想层面、技术层面和艺术层面突破。复习课效益提升中需要反思应试功利和科学素养培养2个问题。     

A New 1D Iodoargentate Chain Based on Heptameric Ag_7I_(13) Building Units Templated by Transition-metalcomplex Cation: Structure,Fluorescence and Visible Light Responding Photocatalytic Property

Using transition-metal-complex cation as the structure-directing agent, a novel one-dimensional(1D) iodoargentate-based hybrid, namely, {[Co(2,2'-bipy)_3]_2(Ag_7I_(11))·3H_2O}_n(1) has been synthesized and structurally characterized. The interesting 1D(Ag_7I_(11))_n~(4n-) chain of 1 is constructed from a heptameric Ag_7I_(13) secondary building unit, in which abundant argentophilic interactions can be observed. Intermolecular C–H···π among [Co(2,2'-bipy)_3]~(2+) cations and C–H···I interactions between [Co(2,2'-bipy)_3]~(2+) cations and(Ag_7I_(11))_n~(4n-) chains contribute to the formation of a 3D network. The optical gap(2.58 eV) based on UV-Vis diffuse-reflectance measurement suggests the semiconductor nature of 1, which implies an efficient photocatalytic degradation activity on organic pollutants under visible light irradiation. As expected, 1 exhibits photocatalytic activity for the degradation of rhodamine B. The luminescence property was also studied.