在线富集离子色谱-质谱联用法同时测定饲料添加剂中的16种有机酸

建立了在线富集方式结合离子色谱-质谱(IC-MS)快速分离分析16种有机酸的方法。离子色谱配备自制富集柱和分离柱对有机酸进行在线富集和分离;质谱采用大气压化学电离源负离子电离方式(APCI^-),在选择离子监控(SIM)模式下对有机酸进行定性和定量分析。采用200 μL大体积进样,在线富集时间为3 min,以NaOH溶液作为淋洗液,梯度洗脱。结果表明,富集柱和分离柱对有机酸有很好的富集分离能力;16种有机酸在30 min内完全洗脱,并在一定浓度范围内线性关系良好;方法检出限(LODs)为0.01~0.22 mg/L;加标回收率为70.6%~110.8%,相对标准偏差(RSD)≤6.3%。该方法样品前处理简单,分离速度快,有机酸检测灵敏度高,适用于多种饲料添加剂样品中有机酸添加剂的检测。     

TurboFlow在线净化/液相色谱-串联质谱法快速测定动物源性食品中聚醚类抗生素的研究

建立了Turbo Flow在线净化/液相色谱-串联质谱法快速同时测定牛奶、鸡肉和鸡蛋中拉沙洛菌素、盐霉素、莫能菌素、甲基盐霉素、马杜霉素和尼日利亚菌素残留的方法。样品提取液经在线净化柱Cyclone-p净化,Thermo Scientific Hypersil-Gold C8(150 mm×2.1 mm,5μm)色谱柱分离,电喷雾正离子模式测定,整个分析过程仅13 min。方法在1~100μg/L范围内呈良好线性关系(r≥0.999),定量下限为1μg/kg,在动物源性食品中3个加标水平下的回收率为71.9%~109.0%,相对标准偏差为1.5%~14.9%。     

流动注射-分光光度法测定自来水中游离氯的研究

设计了游离氯流动注射自动在线检测仪,并研究了仪器的最佳测试条件.该仪器采用改进的N,N-二乙基-1,4-苯二胺(DPD)比色原理,通过流动注射进样技术,结合光电转化、数字信号处理及自动化控制技术,克服了DPD分光光度法中手工操作的缺陷,实现了样品分析的自动化.结果证明,此系统的试剂用量少、测定范围宽(0.05～6.00...     

神府烟煤以及贵阳贫煤分别与木屑掺烧灰沉积特性研究

利用CCD相机和沉积探针组成的在线监测系统，在50 kW下行炉上研究了木屑与神府烟煤以及贵阳贫煤的掺烧灰沉积特性。灰渣沉积过程可分为三个阶段：缓慢增长阶段、快速增长阶段和稳定阶段。烟煤掺烧灰沉积厚度随着木屑掺烧比例的增加而增加，贫煤掺烧灰沉积厚度则随着木屑掺烧比例增加而减小。烟煤中掺烧木屑比例为0、6.7%、15%和22%时，渣层稳定厚度分别为1.37、3.85、11.50、20.56 mm，稳定相对热流密度分别为0.44、0.41、0.30、0.26。贫煤掺烧木屑比例为6.7%、15%和22%时，稳定厚度分别为18.65、10.97和9.78 mm，稳定相对热流密度分别为0.29、0.31、0.33。掺烧木屑之后，灰渣初始层中Ca、K元素显著增加。在相同温度下，随着木屑掺烧比例的增加，灰中熔融相比例增加，因为木屑灰分中含有较多的Na₂O、K₂O等碱金属氧化物，而Al₂O₃、SiO₂等含量较少，降低了灰的熔融温度。     

在线凝胶渗透色谱-气相色谱/质谱法检测茶叶中的153种农药残留

建立了在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析茶叶中153种农药残留的方法。样品用乙腈超声提取,提取液经石墨化炭黑固相萃取柱净化后,经GPC-GC/MS在线净化、分离和检测。方法的加标回收率为73.32%～117.05%,相对标准偏差为0.76%～13.18%。方法的检出限和定量限范围分别为0.0003～0.006 mg/kg和0.001～0.02 mg/kg。该方法样品前处理简单、分析时间短,灵敏度和精密度均符合农药多残留检测技术的要求,适用于茶叶中多种农药残留的检测。     

微波辅助快速制备核-壳型尿苷印迹聚合物及其在线富集应用研究

采用微波辅助加热,以尿苷为模板分子,丙烯酰胺(AA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)为交联剂,快速制备尿苷印迹聚合物,聚合时间大大缩短,仅为传统加热的1/8.采用红外光谱和扫描电镜对印迹聚合物进行表征,结果表明二氧化硅表面成功包覆尿苷印迹壳层;该印迹聚合物颗粒分散均匀,印迹壳层厚度约为100 nm.将该印...     

Single Sample Path-Based Optimization of Markov Chains

Motivated by the needs of on-line optimization of real-world engineering systems, we studied single sample path-based algorithms for Markov decision problems (MDP). The sample path used in the algorithms can be obtained by observing the operation of a real system. We give a simple example to explain the advantages of the sample path-based approach over the traditional computation-based approach: matrix inversion is not required; some transition probabilities do not have to be known; it may save storage space; and it gives the flexibility of iterating the actions for a subset of the state space in each iteration. The effect of the estimation errors and the convergence property of the sample path-based approach are studied. Finally, we propose a fast algorithm, which updates the policy whenever the system reaches a particular set of states and prove that the algorithm converges to the true optimal policy with probability one under some conditions. The sample path-based approach may have important applications to the design and management of engineering systems, such as high speed communication networks.This work was supported in part by     

Controlled Release of the Dithiocarbamate Ligand From A Polypyrrole Polymer. A Basis For On-Line Electrochemicalycontrolled Derivatisation

Abstract

The development of a novel on-line derivatisation scheme is described. the scheme involves use of a conducting polymeric material into which the derivatising agent is incorporated. the properties of the polymer enable electrochemical controlled release of the reagent into flowing solutions.     

Preliminary study on aerosol particle addition calibration method for on-line quantitative analysis of airborne radioactive particles with ICP-MS

An ambient aerosol concentration enrichment system coupled with ICP-MS for real-time monitoring of airborne radioactive particles is now under development. ICP-MS is very sensitive to sample introduction conditions, so it is necessary to develop an easy-use calibration method for on-line quantitative analysis in field application. In this paper, a calibration method using standard solution instead of monodisperse particles was established and validated preliminarily. First of all, four parameters for the method were determined experimentally, including: uptake flow rate and nebulisation efficiency of the Microconcentric nebuliser, nebulisation/transport efficiency of Aridus Desolvating Sample Introduction System, and Relative Sensitivity Factor between ¹⁵⁹?Tb and ¹⁷⁴?Yb. Then, monodisperse terbium nitrate particles were generated by a commercial Vibrating Orifice Aerosol Generator. Continuous aerosols of ytterbium nitrate droplets were nebulised from standard solution. They were mixed together, desolvated through the membrane dryer and introduced into ICP-MS for on-line analysis of terbium nitrate particles. The air sampled from nuclear environment was also introduced into ICP-MS to investigate the effect of flow rate on instrument responses. Finally, atom numbers of ¹⁵⁹?Tb in discrete terbium nitrate particles were determined using the calibration method and compared to the calculated value. Results show that when air flow rate increase from 10?mL?min^?1 to 100?mL?min^?1, the ratio of ¹⁵⁹?Tb ion count to ¹⁷⁴?Yb ion intensity keeps constant although instrument sensitivity decreases by a factor of 25. The relative standard deviation of ¹⁵⁹?Tb atom number measured is better than 18%. The discrepancy with the calculated value could be attributed to the over-estimation of atom number in the particles generated by VOAG because there was some liquid leakage in the VOAG.     

An improved method for the determination of S-Carboxymethyl-L-cysteine in biological fluids with precolumn derivatization and on-line clean-up

Summary In order to follow levels of S-Carboxymethyl-L-cysteine in biological fluids for a period as long as three half-lives after drug administration during pharmacokinetic studies, an improved method for its determination had to be developed. Like the previous one, this method uses a protein precipitation step followed by an O-Phthalaldehyde derivatization step and then an HPLC on-line clean-up. This latter was obtained by means of a switching valve system, including a Nucleosil CN 5 m (3 cm × 4.6 mm i.d.) precolumn and a Spherisorb ODS 5 m (15 cm×4.6 mm i.d.) analytical column. The sensitivity limit was improved to 0.1 g/ml in plasma samples and 0.2 g/ml in urine samples.This method was applied in studies comparing single (0.75 g) and repeated (0.75 g tid) oral administration of the drug to 30 elderly patients and 20 healthy volunteers. Results showed that the half-life was 40% longer in elderly patients than in healthy volunteers, and that area under the plasma concentration versus time curve (AUC) values in elderly patients were twice those obtained with young subjects.