Development,validation of QuEChERS-based method for simultaneous determination of multiclass pesticide residue in milk,and evaluation of the matrix effect

Extraction and quantification of pesticide residue from the milk matrix at or below the established maximum residue limit (MRL) is a challenging task for both analytical chemists and the regulatory institutions to take corrective actions for the human health and safety. The main aim of the study is to develop a simple rapid and less expensive QuEChERS extraction and cleanup method for simultaneous analysis of 41 multiclass pesticide residue in milk by gas chromatography-electron capture detector (GC-ECD), followed by confirmation of the residues with gas chromatography-mass spectrometer (GC-MS). Effect of sorbent type, temperature, spiking concentration, matrix effect (ME), measurement uncertainty (MU), inter- and intra-assay repeatability, reproducibility of recovery, and trueness of the results were investigated to validate the effectiveness of the method. Limit of determination (LOD) and limit of quantitation (LOQ) for all the analytes ranged within 0.001–0.02 and 0.002–0.05 µg mL^?1, respectively. The % recovery of all the pesticides ranged between 91.38 and 117.56% with relative standard deviation (RSD) below 2.79%. The MU for all the analytes was ≤29% of respective LOQs, and except for few pesticides, the ME was largely negative. The method fulfilled all the SANTE guidelines and thus can be extended for routine analysis of multiclass pesticide residue in milk.     

Easy and fast extraction methods to determine organochlorine pesticides in sewage sludge,soil, and water samples based at low temperature

Organochlorine pesticides present in sewage sludge can contaminate soil and water when they are used as either fertilizer or agricultural soil conditioner. In this study, the technique solid–liquid extraction with low temperature purification was optimized and validated for determination of ten organochlorine pesticides in sewage sludge and soil samples. Liquid–liquid extraction with low temperature purification was also validated for the same compounds in water. Analyses were performed by gas chromatography-mass spectrometry operating in the selective ion monitoring mode. After optimization, the methods showed recoveries between 70% and 115% with relative standard deviation lower than 13% for all target analytes in the three matrices. The linearity was demonstrated in the range of 20 to 70 µg L^?1, 0.5 to 60 µg L^?1, and 3 to 13 µg L^?1, for sludge, soil, and acetonitrile, respectively. The limit of quantification ranged between 2 and 40 µg kg^?1, 1 and 6 µg kg^?1, and 0.5 µg L^?1 for sludge, soil, and water, respectively. The methods were used in the study of pesticide lixiviation carried out in a poly vinyl chlorine column filled with soil, which had its surface layer mixed with sludge. The results showed that pesticides are not leached into soil, part of them is adsorbed by the sewage sludge (4–40%), and most pesticides are lost by volatilization.     

撞击流反应器萃取电镀废水中Cr6+的实验研究

以磷酸三丁酯（TBP）为萃取剂,用撞击流反应器对模拟含铬电镀废水中的Cr^6＋进行了萃取脱除实验研究。与相同条件下的传统单级化学萃取相比,撞击流反应器利用两喷嘴的射流作用在两流体相对撞击时获得高效传质区域,能有效强化液液萃取的相际传质过程,其单级萃取率最多可提高20．11％。当萃取剂中TBP的体积分数为10％、相比（有机相与水相的体积比）为1：2、萃取时间为1min、H^＋的浓度为1．0mol／L时,通过实验得出适宜的操作条件为：喷嘴间距离为喷嘴直径的3．4倍,搅拌转速600r／min,萃取温度30—40℃,在此条件下Cr^6＋的萃取率为31．5％。     

酸化-萃取法处理丁辛醇废水

采用酸化-萃取法处理齐鲁石化公司第二化肥厂的丁辛醇废水（简称废水）,用硫酸调节废水的pH,以该厂产品异辛醇为萃取剂,考察了各种因素对萃取效率的影响,得出较佳工艺条件：废水的pH为2．5,废水与萃取剂的体积比为4,废水温度为10℃,废水与萃取剂混合时的振摇时间为60s,萃取相和萃余相的静置分离时间为10min。在该条件下对COD为42244mg/L的废水进行二级错流萃取,COD去除率为86．82％。该法可实现对废水进行处理和资源回收的双重目的。     

水中有机磷农药分析前处理方法探讨

分别采用液-液萃取、固相萃取前处理方法,提取水中10种常见的有机磷农药,对比了这两种提取方法的测定结果、经济成本、花费时间及对环境的影响,建议逐步用固相萃取法取代液？液萃取法提取水中有机磷农药。     

超声波提取土壤中的半挥发性有机物

用二氯甲烷索氏提取法对比多种萃取剂超声波提取法测定标准土壤样品回收率的结果,以实验得出二氯甲烷超声波提取法的样品加标回收率及相对标准偏差。结果表明,二氯甲烷超声萃取法提取土壤中的半挥发性有机物的时效性,准确性能够满足监测分析的要求。     

氟苯生产废水处理及资源化技术

采用酸化、萃取、反萃、除氟、电催化氧化技术处理氟苯生产废水（简称废水）。工艺条件为：以硫酸为酸化剂,pH小于等于1;萃取温度10～25℃,搅拌时间大于4min,油水比（萃取剂与废水的体积比）1：4．0;反萃碱油比（NaOH溶液体积与油相体积比）1：3,NaOH质量分数10％;除氟时先加入2倍理论计算量的氯化钙、后加入氧化钙调pH至7～8;电催化氧化时粒子群电催化反应器槽电流2．0～2．5A,停留时间40～60min。处理后废水的COD、苯酚、F^-、石油类去除率分别高于99．3％,99．9％,99．8％,99．9％,苯酚回收率高于93．5％;出水COD、苯酚、F^-、石油类的浓度低于GB8978—1996《污水综合排放标准》中的一级排放标准。     

Sonolytic reactions of phenanthrene in organic extraction solutions

Ultrasonic extraction is a common method used to extract semi-volatile and nonvolatile organic compounds such as polycyclic aromatic hydrocarbons (PAHs) from solid matrices. However, ultrasonic energy has been suspected to lead to undesired reactions of the solute and thus affect qualitative and quantitative results. In this paper, sonolytic reactions of phenanthrene in common organic extraction solutions were examined using a 20 kHz ultrasonic probe under conditions commonly used for ultrasonic extraction. Extraction parameters including phenanthrene concentration, solvent type, pulse length, and sonication time were investigated. Hexane:acetone (1:1 V/V) resulted in less phenanthrene degradation than dichloromethane (DCM):acetone (1:1 V/V). Initial solute concentration, length of sonication time, and solvent type affected the degradation of phenanthrene. Reaction byproducts including methylphenanthrene and methylnaphthalene detected after sonication indicate that phenanthrene reacts by both direct pyrolysis and reaction with methyl or ethyl radicals formed from solvent pyrolysis.     

用络合萃取法对磺酸型有机废水进行预处理的研究

采用络合萃取法对磺酸型有机废水进行预处理，研究了萃取过程中废水ＰＨ、萃取睡稀释凤加量对废水萃取效果的影响。实验结果表明，当ＰＨ为１．０时，萃取剂和稀释剂按废水；萃取剂；稀释剂＝１００：１０：２５的投加，可取得较好的效果。萃取后的络合相经碱解分离即可回收萃取剂，萃取剂循环使用１０次，废水的ＣＯＤ去除率无下降趋势。     

Dispersive solid phase extraction of chlorophenols using carbon-coated magnetic nanoparticles

Abstract

Carbon-coated magnetic nanoparticles were modified with cationic surfactant and used for the dispersive solid phase extraction of chlorophenols from aqueous samples. Surfactant adsorbed on the surface of the nanoparticles resulted in mixed hemimicelles for high extraction efficiency of chlorophenols. Under optimized conditions, calibration curves were linear from 0.5–20?mg L^?1 for analytes with limit of detection between 0.2 and 0.4?mg L^?1. The method was applied to extraction of chlorophenols from tap water, well water and industrial effluent. Recoveries were in the range of 94.0–99.4%, suggesting that sample matrix had little effect on the yields of extraction.