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建立了固相萃取-超高效液相色谱-串联质谱法(SPE-UPLC-MS/MS)同时测定牛奶中苄青霉素、邻氯青霉素、氨苄青霉素3种青霉素残留的分析方法。以自制的共价三嗪骨架(CTFs)材料作为固相萃取吸附剂,对影响固相萃取柱效率的吸附剂填充量、洗脱剂种类和用量及上样速率等主要因素进行了优化;同时对样品的提取和净化条件进行了考察。在3 mL/min的样品流速下,采用60 mg CTFs吸附剂和6 mL纯乙腈洗涤液达到了最佳的萃取效果。以0.1%甲酸水溶液-乙腈作为流动相进行梯度洗脱,在Waters ACQUITY UPLC BEH C18色谱柱上分离,电喷雾正离子(ESI+)模式下以动态多反应监测(MRM)采集数据,外标法定量。3种目标分析物的线性回归方程相关系数均大于0.999,检出限(LOD)为0.05~0.10 μg/kg(信噪比S/N=3),定量限(LOQ)为0.1~0.4 μg/kg(S/N=10),加标回收率为84.9%~94.1%,相对标准偏差(RSD, n=5)为1.66%~3.27%。此外,共价三嗪骨架材料与目标物的作用机理研究表明,主客体分子间存在π-π相互作用和氢键作用等多重相互作用,使该吸附剂可成功用于牛奶中青霉素的富集和净化。该方法具有精密度较高、重复性较好、分离度高、分析时间短等优点,可适用于牛奶中青霉素定性定量测定。 相似文献
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建立了测定草莓中鞣花酸含量(包括游离鞣花酸和总鞣花酸)的超高效液相色谱-质谱联用(UPLCMS/MS)分析方法。草莓中游离鞣花酸在酸性条件下用甲醇提取,经C18分散固相萃取净化后可直接测定;总鞣花酸经酸性水解呈游离态再经分散固相萃取净化后进行测定。净化液经C18色谱柱分离,以甲醇和0.5%甲酸水为流动相进行梯度洗脱,电喷雾负离子(ESI-)模式电离,超高效液相色谱-质谱法(UPLC-MS/MS)测定,外标法定量。结果表明:在10~500 ng/m L浓度范围内鞣花酸的线性关系良好,相关系数为0.998 1,游离鞣花酸的定量下限为0.5 mg/kg,总鞣花酸的定量下限为5.0 mg/kg。在低、中、高3个加标浓度的回收实验中,游离鞣花酸的加标回收率为86.7%~113.6%,相对标准偏差均小于10%。该方法操作简单,灵敏度高,准确性好,适用于草莓中鞣花酸的测定。 相似文献
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This paper analyses the reverse recovery characteristics and
mechanism of SiGeC p-i-n diodes. Based on the integrated systems
engineering (ISE) data, the critical physical models of SiGeC diodes
are proposed. Based on heterojunction band gap engineering, the
softness factor increases over six times, reverse recovery time is
over 30% short and there is a 20% decrease in peak reverse
recovery current for SiGeC diodes with 20% of germanium and
0.5% of carbon, compared to Si diodes. Those advantages of SiGeC
p-i-n diodes are more obvious at high temperature. Compared to
lifetime control, SiGeC technique is more suitable for improving
diode properties and the tradeoff between reverse recovery time and
forward voltage drop can be easily achieved in SiGeC diodes.
Furthermore, the high thermal-stability of SiGeC diodes reduces the
costs of further process steps and offers more freedoms to device
design. 相似文献
15.
Based on the connection between the tent map and the saw tooth map or Bernoulli map, a novel method for the initial-condition estimation of the tent map is presented. In the method, firstly the symbolic sequence generated from the tent map is converted to the forms obtained from the saw tooth map and Bernoulli map, and then the relationship between the symbolic sequence and the initial condition of the tent map can be obtained from the initial-condition estimation equations, which can be easily obtained, hence the estimation of the tent map can be achieved finally. The method is computationally simple and the error of the estimator is less than 1/2N. The method is verified by software simulation. 相似文献
16.
A Novel Fully Depleted Air AlN Silicon-on-Insulator Metal--Oxide--Semiconductor Field Effect Transistor 下载免费PDF全文
A novel fully depleted air A1N silicon-on-insulator (SOD metai-oxide-semiconductor field effect transistor (MOS- FET) is presented, which can eliminate the self-heating effect and solve the problem that the off-state current of SOI MOSFETs increases and the threshold voltage characteristics become worse when employing a high thermal conductivity material as a buried layer. The simulation results reveal that the lattice temperature in normal SOI devices is 75K higher than the atmosphere temperature, while the lattice temperature is just 4 K higher than the atmosphere temperature resulting in less severe self-heating effect in air A1N SOI MOSFETs and A1N SOI MOSFETs. The on-state current of air A1N SOI MOSFETs is similar to the A1N SOI structure, and improves 12.3% more than that of normal SOI MOSFETs. The off-state current of A1N SOI is 6. 7 times of normal SOI MOSFETs, while the counterpart of air A1N SOI MOSFETs is lower than that of SOI MOSFETs by two orders of magnitude. The threshold voltage change of air A1N SOl MOSFETs with different drain voltage is much less than that of A1N SOI devices, when the drain voltage is Mased at 0.8 V, this difference is 28mV, so the threshold voltage change induced by employing high thermal conductivity material is cured. 相似文献
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含环碳酸酯基新型聚合物载体的合成及固定化葡萄糖淀粉酶研究 总被引:13,自引:0,他引:13
碳酸亚乙烯酯(VCA)分子中的反应性环碳酸酯基可于温和条件下与氨基发生反应形成稳定的氨基甲酸酯.利用这一性质,将含-NH2基团的酶分子直接以σ键的形式固定于含有环碳酸酯基的聚合物载体上.本文通过反相悬浮聚合,以液体石蜡为介质,VCA为反应性单体,甲基丙烯酸-β-羟乙酯(HEMA)及丙烯酸羟丙酯(HPA)为亲水性共聚单体,合成出一系列交联树脂聚合物.以此聚合物为载体对葡萄糖淀粉酶进行固载实验,表现出良好的固定化性能.同时,固定化酶的稳定性也有所提高. 相似文献
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利用脒基硫脲和3,5-二羟基苯甲酸制备出了一种新型的加合物(C2H7N4S)+·(C7H5O4)-,用X射线单晶衍射试验方法测定其晶体结构.结果表明,晶体属单斜晶系,P21/n空间群,其中a=0.72303(1)nm,b=1.42970(3) nm,c=1.07991(2)nm,β=91.591(2)°,Z=4,R1=0.0303, wR=0.0823(I>2σ(I)).在标题化合物的晶体结构中,3,5-二羟基苯甲酸通过羧基和羟基的O-H…O氢键头尾相连形成了沿b轴无限延伸的"Z"型链,脒基硫脲通过氢键的缔合和静电相互作用连接3,5-二羟基苯甲酸的"Z"型链构成了3D超分子氢键网络结构. 相似文献
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合成了2,2’-二(4-羟基苯基)丙烷为主体分子的四丁基铵包合物, [(n-C4H9)4N]+8226;[(C15H15O2)2H]-, 并通过单晶X射线衍射法对其进行了晶体结构测定, 发现该包合物的晶体存在两种同质异晶体. 结果表明, 晶型1属单斜晶系, C2/c空间群, 晶胞参数a=2.8199(2) nm, b=0.92730(8) nm, c=2.1450(3) nm, β=130.050(1)°, Z=4, R1=0.0771, wR2=0.2452; 晶型2属三斜晶系, P`1空间群, 晶胞参数a=1.0895(1) nm, b=1.2331(2) nm, c=1.7244(2) nm, α=108.137(2)°, β=94.458(2)°, γ=100.172(2)°, Z=2, R1=0.0697, wR2=0.2176. 晶型1中2,2’-二(4-羟基苯基)丙烷阴离子的氢键链构成管道式主体晶格, 正四丁基铵阳离子被包合在这些管道中; 晶型2中2个独立的2,2’-二(4-羟基苯基)丙烷阴离子分别形成氢键主体层, 它们交替排列并与夹在其间的正四丁基铵阳离子形成类三明治层状包合物. 相似文献
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本文设计合成了一种对硝基偶氮水杨醛吖嗪pH传感器S1。通过紫外可见分光光度法研究了传感器S1与八种不同阴离子的识别性能。通过向10%HEPES缓冲液(DMSO/HEPES=9∶1,V/V,pH=5.63)的S1中分别加入F~-、Cl~-、Br~-、I~-、AcO~-、SO_4~(2-)、NO_3~-、H_2PO_4~-等阴离子后,发现F~-、AcO~-、H_2PO_4~-的加入使得S1在584、614、622nm处的吸收峰增强,溶液颜色由淡黄色转变为蓝色,同时其它离子的加入无上述现象。Job曲线测定了S1与F~-、AcO~-、H_2PO_4~-的化学计量比均为1∶1,及最低检测限分别为0.39,2.60和12.5μM。通过布朗斯特酸碱反应及密度泛函理论计算说明S1与F~-、AcO~-、H_2PO_4~-之间可能是脱质子化作用。由此可见传感器S1在溶液体系中是一种颜色可调的可视化传感器。 相似文献