Experimental approaches for the estimation of uncertainty in analysis of trace inorganic contaminants in foodstuffs by ICP-MS

Total Diet Studies to estimate dietary exposure to food contaminants need to evaluate laboratory measurements data variance. In this process it is critical that data from analytical methods are reliable to correctly scrutinize and compare values over time and between countries. In Europe it is widely recognized that the evaluation of measurement uncertainty is an important parameter when assessing the sources of analytical data variability. Two approaches are considered to estimate uncertainty in analytical measurement. Arsenic, Lead, Chromium and Cadmium, content in several food matrix determined by Inductively Coupled Mass Spectrometry (ICP-MS) microwave digestion assisted, are used as examples. The aim of the present research work is to compare both approaches accepted by Eurolab and GUM: Mathematical modeling to assess uncertainty components based on a classical model (bottom up) and an empirical method (top down), based on either experimental data obtained from a single laboratory validation data or inter-laboratory data from Proficiency Testing schemes. Relative expanded uncertainty calculated by both approaches agree when U (%) <20%. These values are concordant with RSD_R reported in collaborative studies of EN 15763 (2009), which were assumed as target uncertainty. The top down approach described is simple and easy to use when compared with the mathematical modeling approach providing considerable benefits to those who assess data produced by several laboratories.     

Analysis of triclosan and 4n‐nonylphenol in Colombian reservoir water by gas chromatography‐mass spectrometry

In this work were determined triclosan and 4n‐nonylphenol in water from a reservoir that is used to provide water to a purification plant in an important city in Colombia. The analytical methodology was validated using solid‐phase extraction and analysis by gas chromatography‐mass spectrometry (GC‐MS). The analysis by GC‐MS showed good linearity in the range of 0.05–5 μg/L for both compounds. Recoveries from 79 to 109% and standard deviations of 2.5–7.7 for low concentrations and from 3.8 to 9.6 (n = 5) for high concentrations were obtained for both compounds. In Colombia, this is the first time that these compounds have been analysed in water supplying of a drinking water treatment plant. The validated method was applied to the analysis of 27 samples collected in August 2010 in 11 locations from the reservoir and in the influent and effluent of the drinking water treatment plant. In total, seven samples were found to contain triclosan.     

吸附剂针对性净化-气相色谱-三重四极杆串联质谱测定油茶果中55种持久性有机污染物

建立了针对性净化与气相色谱-串联质谱相结合的方法,测定油茶果不同部位中16种多环芳烃、18种多氯联苯和21种有机氯共55种持久性有机污染物（POPs）。油茶籽仁、油茶外种皮和油茶壳样品采用乙腈提取,氯化钠盐析,离心分层后,分别向提取液中加入无水硫酸镁和PSA、C18、Florisil、Si、SCX、NANO Carb与Pesticarb等 7种吸附剂进行多管漩涡振荡分散固相净化比较,多反应监测模式检测。结果表明,55种持久性有机污染物在20~1 000 μg/L浓度范围内具有良好的线性关系,检出限为0.25~65.50 μg/kg,定量限为0.84~218.34 μg/kg,加标回收率为69.1%~138.2%。应用本方法检测来自湖南、江西和浙江共54份油茶的POPs,从油茶籽仁检出萘、狄氏剂、芴、毒杀芬、菲、α-六六六和苊萘嵌戊烷（4.36~566.26 μg/kg）;外种皮检出萘、芴、菲、毒杀芬、α-六六六和苊萘嵌戊烷（3.62~1 109.43 μg/kg）;油茶壳检出萘、毒杀芬、芴和菲（5.13~703.57 μg/kg）。该方法适用于油茶果不同部位持久性有机污染物的检测,对其他油料作物的POPs分析也具有一定的参考价值。     

基于遗传算法的18Ni300钢持久性能的神经网络预测

本文研究时效温度和时效时长对18Ni300马氏体时效钢持久性能的影响,对经过不同时效处理的18Ni300钢进行不同高温条件下的持久性能测试。结果表明:在时效温度480℃时,时效处理5h的18Ni300钢的持久性能较时效处理5h有明显提高,且经不同时效处理的马氏体时效钢的持久性能随测试温度的增加而逐渐下降。从模型泛化能力和预测精度出发,根据有限的持久性实验数据,基于遗传算法构建了预测18Ni300钢持久性能的3-12-1型GA-BP神经网络模型。18Ni300钢持久性能的GA-BP网络预测结果与试验数据的吻合性较好,这说明所构建的18Ni300钢的持久性能GA-BP神经网络模型的预测精度和可靠性较高,可有效用于时效处理对18Ni300钢持久性能的预测。     

THE PHYSICAL MODEL AND MATH MODEL OF CONTACT FAILURE ON SMALL CURRENT CONTACTS UNDER MECHANICAL ACTIONS

Based on the experimental results of the references [1 ] and [2], i.e., the contact re-sistance increases due to the contaminants formed on contact surface with the operating cycles,the physical model and math model of contact failure on small current contacts under mechanicalactions are proposed through deep theoretical analysis in this paper.     

超声和多种技术联用在废水处理中的应用

超声降解技术对废水中的各类有机物具有广泛的适应性,在废水处理中得到了广泛的关注。本文介绍了超声降解的机理和影响因素。超声降解技术和光催化、电催化、化学氧化、生物技术联用可以提高降解有机废水的效率。     

便携式GC-MS在应急监测中的应用

随着我国经济的高速发展,企业生产的不断扩张,企业的环境突发事故的多变性,对现场监测提出了更高的要求。建立便携式GC-MS,由于其体积小,分析精度高,非常适合于现场挥发性有机物的分析,在国内已被成功用于多起现场环境应急监测工作,本文以一次监测实例说明通过充分利用该仪器快速检测极低浓度挥发性有机污染物的功能,可将之进一步应用于被污染环境空气的实时现场监测,从而为复杂情况下环境污染源的快速排查工作提供强有力的技术支持。     

食品中多氯联苯检测技术研究进展

多氯联苯(polychlorinated biphenyls, PCBs)是由一个或多个氯原子取代联苯分子中氢原子而形成的一类有机化合物的总称,具有持久性、高富集性和生物毒性等特点。普通人群摄入PCBs的主要途径是通过食物摄入,尤其是动物源性食品。PCBs可能会对人类和动物神经发育、生殖、消化、免疫等系统造成不利影响,对人类身体健康具有严重危害。本文对近5年食品中PCBs检测技术研究进行了综述,系统地梳理了样品前处理及各种测定技术的现状,对这些方法的创新性、局限性等进行了总结,并对食品中PCBs检测技术未来的发展进行了展望,为进一步降低和控制食品中的PCBs含量提供了参考。     

持久性有机污染物机械化学无害化处理的研究进展

机械化学处理方法是目前最有商业化应用前景的持久性有机污染物(POPs)无害化处理技术之一, 尤其适宜于发展中国家的偏远地区使用。详细介绍了POPs机械化学处理研究起源与现状, 分析了工艺原理及优点, 提出下一步研究工作的重点是强化POPs机械化学反应机理及产物结构的研究, 明确中间及最终产物的结构形态, 确认工艺安全性与有效性, 消除疑虑, 推动工艺的商业化应用。     

The Evidence for Effective Inhibition of INa Produced by Mirogabalin ((1R,5S,6S)-6-(aminomethyl)-3-ethyl-bicyclo [3.2.0] hept-3-ene-6-acetic acid), a Known Blocker of CaV Channels

Mirogabalin (MGB, Tarlige^®), an inhibitor of the α₂δ-1 subunit of voltage-gated Ca²⁺ (Ca_V) channels, is used as a way to alleviate peripheral neuropathic pain and diabetic neuropathy. However, to what extent MGB modifies the magnitude, gating, and/or hysteresis of various types of plasmalemmal ionic currents remains largely unexplored. In pituitary tumor (GH₃) cells, we found that MGB was effective at suppressing the peak (transient, I_Na(T)) and sustained (late, I_Na(L)) components of the voltage-gated Na⁺ current (I_Na) in a concentration-dependent manner, with an effective IC₅₀ of 19.5 and 7.3 μM, respectively, while the K_D value calculated on the basis of minimum reaction scheme was 8.2 μM. The recovery of I_Na(T) inactivation slowed in the presence of MGB, although the overall current–voltage relation of I_Na(T) was unaltered; however, there was a leftward shift in the inactivation curve of the current. The magnitude of the window (I_Na(W)) or resurgent I_Na (I_Na(R)) evoked by the respective ascending or descending ramp pulse (V_ramp) was reduced during cell exposure to MGB. MGB-induced attenuation in I_Na(W) or I_Na(R) was reversed by the further addition of tefluthrin, a pyrethroid insecticide known to stimulate I_Na. MGB also effectively lessened the strength of voltage-dependent hysteresis of persistent I_Na in response to the isosceles triangular V_ramp. The cumulative inhibition of I_Na(T), evoked by pulse train stimulation, was enhanced in its presence. Taken together, in addition to the inhibition of Ca_V channels, the Na_V channel attenuation produced by MGB might have an impact in its analgesic effects occurring in vivo.