火龙果果皮色素的提取及稳定性研究

研究了火龙果果皮色素提取的最佳条件、提取液的稳定性和各种添加剂对提取液稳定性的影响。     

枇杷核中提取苦杏仁甙的研究

研究了3个枇杷品种的出核率，利用高效液相色谱检测苦杏仁甙的含量，以及从枇杷核中提取苦杏仁甙的工艺。结果表明，3个品种烘干后核的得率存在显著差异，干核的年产量很大，有综合开发利用价值；提取溶剂以乙醇为好，最合理的工艺组合为：在原料中按料液比1：10加入浓度为80％的乙醇，在65℃时回流提取50min。在40℃功率为80W的条件下超声处理25min。合理选择品种是提高苦杏仁甙得率的关键。     

采油厂HSE监督检查管理系统创建实践研究

本文根据采油厂生产过程风险特点,以生产单元为对象,通过建立全员参与的HSE监督检查体系,实现对采油厂HSE监督检查标准的统一规范,利用开发的HSE监督检查信息集成平台,创建完成采油厂HSE监督检查管理系统。在大庆油田第五采油厂的应用实践显示,其能为采油厂带来巨大的风险管理效益,是全面落实直线与属地HSE责任的有效载体。对于采油厂有效实施HSE监督检查具有重大意义,是HSE管理制度的一种创新。     

Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

• Isotope dilution method was developed for the determination of 27 PPCPs in water. • The established method was successfully applied to different types of water samples. • The correction effect of corresponding 27 ILSs over 70 d was investigated. • Benefit of isotopic dilution method was illustrated for three examples. Pharmaceuticals and personal care products (PPCPs) are a unique group of emerging and non-persistent contaminants. In this study, 27 PPCPs in various water samples were extracted by solid phase extraction (SPE), and determined by isotope dilution method using liquid chromatography coupled to tandem triple quadruple mass spectrometer (LC-MS/MS). A total of 27 isotopically labeled standards (ILSs) were applied to correct the concentration of PPCPs in spiked ultrapure water, drinking water, river, effluent and influent sewage. The corrected recoveries were 73%–122% with the relative standard deviation (RSD)<16%, except for acetaminophen. The matrix effect for all kinds of water samples was<22% and the method quantitation limits (MQLs) were 0.45–8.6 ng/L. The developed method was successfully applied on environmental water samples. The SPE extracts of spiked ultrapure water, drinking water, river and wastewater effluent were stored for 70 days, and the ILSs-corrected recoveries of 27 PPCPs were obtained to evaluate the correction ability of ILSs in the presence of variety interferences. The recoveries of 27 PPCPs over 70 days were within the scope of 72%–140% with the recovery variation<37% in all cases. The isotope dilution method seems to be of benefit when the extract has to be stored for long time before the instrument analysis.     

一种简便高效的土壤石油烃提取方法的建立

通过开展单因子实验与正交实验,考察不同参数下超声萃取法对土壤中总石油烃(TPH)的提取效率,并对比了超声萃取法、超声-索氏萃取法及传统索氏萃取法对不同原油污染土壤的提取效果。结果表明:超声萃取法的最优工作参数为20 m L二氯甲烷,超声10 min,4000 r/min离心10 min,萃取4次。3种提取方法中,超声萃取法对石油烃平均回收率最高,为100.95%,而传统的索氏萃取法最低,仅为94.54%。可见,超声萃取法操作简单,效率高,可广泛用于土壤中总石油烃含量的提取测定。     

流体剪切与超声空化破解剩余污泥的参数优化

为提高剩余污泥的破解效果并降低能耗,采用FS（fluid shear,流体剪切）、UC（ultrasonic cavitation,超声空化）、FS和UC联合工艺（FS-UC,UC-FS）破解剩余污泥,并应用单因素试验结合响应面法对联合工艺进行优化.结果表明:FS对剩余污泥破解效果一般,只在开始阶段具有较好效果,随作用时间延长,破解效果未有显著提高甚至下降.UC对剩余污泥破解效果明显,随作用时间延长,破解效果显著提升,但能耗也随之增大,EDR（energy disintegration ratio,效能比）明显下降.相同作用时间下,UC破解效果优于FS破解效果,UC破解剩余污泥的DD_COD（degree of disintegration,破解率）与EDR均明显高于FS方法.单因素试验得出的较优FS作用时间范围为2~8 min,较优UC作用时间范围为5~15 min.响应面法试验结果显示,联合工艺的剩余污泥破解效果和能量利用率均优于单一方法,联合工艺中FS-UC工艺的破解效果优于UC-FS工艺.FS-UC工艺的最佳参数:FS处理5.6 min再UC处理15.0 min,该条件下剩余污泥实际DD_COD为50.8%,EDR为26.8%.UC-FS工艺的最佳参数:先UC作用15.0 min再FS作用7.8 min,该条件下剩余污泥实际DD_COD为36.5%,EDR为17.1%.研究显示,以DD_COD和EDR为指标,4种工艺的高效性顺序为FS-UC > UC-FS > UC > FS,其中FS-UC工艺具有能耗低、破解效率高的特点,是4种工艺中剩余污泥破解效果最好的一种工艺.      

电晕放电辐射信号的特征提取和模式识别方法研究

目的研究电晕放电辐射信号的特征提取和模式识别方法。方法在分析信号特征提取方法的基础上,对实测的电晕放电辐射信号特征提取,利用概率神经网络开展电晕放电辐射信号目标识别,检验特征提取的有效性。结果以奇异值作为输入特征量的PNN在整体上效果更优,稳定性好,对两类不同放电辐射信号的正确识别率均可达到80%以上,并且当输入特征量个数达到10个时,对实测样本的正确识别率均达到了最高值。电晕放电的正确识别率为96.7%,火花放电的正确识别率为93.3%。结论该方法能基本满足实际放电信号的识别应用。     

沉积物中雌激素及壬基酚、辛基酚、双酚A的测定

近些年来雌激素及烷基酚类化合物由于其对水生生物的内分泌干扰作用越来越受到广泛关注.沉积物作为环境中有机污染物的重要储存库,研究目标物在其中的浓度分布对于探明此类物质在环境中的迁移转化具有重要意义.但沉积物中基质组成复杂而雌激素又痕量存在,这增加了前处理的难度.本研究从雌激素及烷基酚类化合物的理化性质入手,采用碱液提取、液液萃取和LC-MS/MS分析测定沉积物样品中的雌激素及壬基酚、辛基酚、双酚A.结果表明,经过优化的方法对7种目标物的回收率介于61.9%～93.7%之间.该方法能有效去除沉积物中那些不溶于强碱和既溶于酸又溶于碱的有机污染物,同时操作简单、成本低,但回收率高、检出限低,可广泛适用于河流沉积物样品及土壤样品的前处理.     

Application of comprehensive two-dimensional gas chromatography with mass spectrometric detection for the analysis of selected drug residues in wastewater and surface water

Pharmaceutical residues have become tightly controlled environmental contaminants in recent years, due to their increasing concentration in environmental components. This is mainly caused by their high level of production and everyday consumption. Therefore there is a need to apply new and sufficiently sensitive analytical methods, which can detect the presence of these contaminants even in very low concentrations. This study is focused on the application of a reliable analytical method for the analysis of 10 selected drug residues, mainly from the group of non-steroidal anti-inflammatory drugs (salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, acetaminophen, caffeine, naproxen, mefenamic acid, ketoprofen, and dicofenac), in wastewaters and surface waters. This analytical method is based on solid phase extraction, derivatization by N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and finally analysis by comprehensive two-dimensional gas chromatography with Time-of-Flight mass spectrometric detection (GC×GC- TOF MS). Detection limits ranged from 0.18 to 5 ng/L depending on the compound and selected matrix. The method was successfully applied for detection of the presence of selected pharmaceuticals in the Svratka River and in wastewater from the wastewater treatment plant in Brno-Modrice, Czech Republic. The concentration of pharmaceuticals varied from one to several hundreds of ng/L in surface water and from one to several tens of μg/L in wastewater.     

TiO2 nanotubes as solid-phase extraction adsorbent for the determination of polycyclic aromatic hydrocarbons in environmental water samples

An analytical method based on TiO2 nanotubes solid-phase extraction (SPE) combined with gas chromatography (GC) was established for the analysis of seven polycyclic aromatic hydrocarbons (PAHs): acenaphtylene, acenaphthene, anthracene, fluorene, phenanthrene, fluoranthene and pyrene. Factors a ecting the extraction e ciency including the eluent type and its volume, adsorbent amount, sample volume, sample pH and sample flow rate were optimized. The characteristic data of analytical performance were determined to investigate the sensitivity and precision of the method. Under the optimized extraction conditions, the method showed good linearity in the range of 0.01–0.8 g/mL, repeatability of the extraction (RSD were between 6.7% and 13.5%, n = 5) and satisfactory detection limits (0.017–0.059 ng/mL). The developed method was successfully applied to the analysis of surface water (tap, river and dam) samples. The recoveries of PAHs spiked in environmental water samples ranged from 90% to 100%. All the results indicated the potential application of titanate nanotubes as solid-phase extraction adsorbents to pre-treat water samples.