Development and application of LC–APCI–MS method for biomonitoring of animal and human exposure to imidacloprid

Imidacloprid (IMI) is a relatively new neuro-active neonicotinoid insecticide and nowadays one of the largest selling insecticides worldwide. In the present study a LC–APCI–MS based method was developed and validated for the quantification of imidacloprid and its main metabolite 6-chloronicotinic acid (6-CINA) in urine and hair specimens. The method was tested in biomonitoring of intentionally exposed animals and subsequently applied for biomonitoring of Cretan urban and rural population.     

Determination of Steroid Estrogens in Wastewater Treatment Plant of A Controceptives Producing Factory

Steroid estrogens such as estrone (E1), 17β-estradiol (E2), estriol (E3), and 17α-ethynylestradiol (EE2) have been suspected to be the main contaminants, which can affect the endocrine system of animals. Many authors have investigated these chemicals in the domestic wastewater treatment plants (WTP). However, wastewater from industries producing steroid contraceptives has not got ample attention. From the environmental point of view, the four steroids are very significant because even very low concentrations (ng/L) can cause reproductive disturbances in human, livestock and wildlife. The main purpose of the present investigation was to develop an analytical method for the determination of the four steroid estrogens present in WTP of a pharmacy factory, mainly producing contraceptive medicine in Beijing, China. Analysis was performed by solid-phase extraction (SPE) system and liquid chromatography combined with tandem mass spectrometry (LC/MS/MS). The average recoveries from effluent samples ranged from 88% to 103% and the precision of the method ranged from 9% to 4%. Based on 0.5-L wastewater samples, the limit of quantification (LOQ) was determined at 0.7 ng/L for E1, 0.8 for E2, 0.9 ng/L for E3, and 0.5 ng/L for EE2 in influent, and 1.0 ng/L for E2 and EE2, and 2.0 ng/L for E1 and E3 in effluent. In the influent samples, average concentrations of 80, 85, 73 and 155 ng/L were determined for E1, E2, E3 and EE2, respectively, showing that they were removed in this WTP to the extent of 79, 73, 85 and 67%, respectively.     

固相萃取-气质联机测定水中嗅味物质2-甲基异茨醇和土霉素

分别利用固相萃取剂XAD-2树脂和C18SEP柱富集,二氯甲烷洗脱,固相萃取装置浓缩,通过气质联机(GC/MS)测定了水中土霉化合物MIB和Geosmin。该方法重现性好,相对标准偏差5.4%~7.0%,回收率80%~92%,MIB和Geosmin检出限分别为5ng/L和2ng/L。两种固相萃取剂对MIB和Geosmin吸附效率相当,吸附效率不受嗅味物质浓度影响,但当水溶液中其它有机质增多时,C18SPE的回收率明显下降。利用该方法对不同培养时间的放线菌代谢产物进行了测定,培养25天后代谢产物MIB和Geosmin的浓度达到200ng/L和130ng/L。     

Pyrolysis of waste animal fats in a fixed-bed reactor: Production and characterization of bio-oil and bio-char

Several animal (lamb, poultry and swine) fatty wastes were pyrolyzed under nitrogen, in a laboratory scale fixed-bed reactor and the main products (liquid bio-oil, solid bio-char and syngas) were obtained. The purpose of this study is to produce and characterize bio-oil and bio-char obtained from pyrolysis of animal fatty wastes. The maximum production of bio-oil was achieved at a pyrolysis temperature of 500 °C and a heating rate of 5 °C/min. The chemical (GC–MS analyses) and spectroscopic analyses (FTIR analyses) of bio-oil showed that it is a complex mixture consisting of different classes of organic compounds, i.e., hydrocarbons (alkanes, alkenes, cyclic compounds…etc.), carboxylic acids, aldehydes, ketones, esters,…etc. According to fuel properties, produced bio-oils showed good properties, suitable for its use as an engine fuel or as a potential source for synthetic fuels and chemical feedstock. Obtained bio-chars had low carbon content and high ash content which make them unattractive for as renewable source energy.     

吹扫捕集与气相色谱-质谱联用测定饮用水和地表水中挥发性有机污染物

报道了Trap I(VOCARB 4000)柱捕集水中挥发性有机污染物的性能和条件,建立了吹扫捕集和气相色谱-质谱联用测定饮用水和地表水样中25种挥发性有机污染物的分析方法.水样的加标回收率在90%～110%之间,最低检测限在0.04～0.85μg/L之间,20μg/L的挥发性有机物标准溶液经重复6次测定,其相对标准偏差基本小于5.0%.该方法已成功地运用于饮用水和地表水中挥发性有机污染物的测定,结果令人满意.     

用Ames试验检测水源水和自来水中的遗传毒性

用微伤寒沙门氏菌／哺乳动物微粒体酶系的Ａｍａｅｓ试验,研究了不同季节物水源水及管网自来水中的遗传毒性,以ＸＡＤ２树脂为吸附剂,以丙酮－甲醇的混合液为洗脱液,浓率水样中的有机物,并对部分阳性水样进行有机成分的定性分析。结果发现：１３个水样中有７个样品在淡需要代谢活化系统Ｓ９的情况下,可诱导鼠伤寒沙门氏菌碱基移码型菌株的回复突变;不同水样在不同季节不同的诱导作用;同时通过ＧＣ／ＭＳ方法分析,发现阳性水     

噬菌体MS2作为水中肠道病毒指示生物的特征及其影响因素

噬菌体MS2作为潜在的水中肠道病毒指示生物,已逐渐成为回用水微生物学安全评价指标的主要研究方向之一。在此,阐述噬菌体MS2作为水中肠道病毒指示生物的主要特征,并介绍噬菌体MS2作为水中肠道病毒指示生物应用的影响因素。     

加速溶剂萃取-固相萃取/超高效液相色谱-串联质谱法测定沉积物中5种微囊藻毒素

建立了加速溶剂萃取-固相萃取/超高效液相色谱-串联质谱法同时测定沉积物中5种微囊藻毒素(MC-LR、MC-RR、MC-LW、MC-LF、MC-YR)的方法。选择甲醇-水(1∶4,V/V)为ASE萃取溶剂,萃取温度和萃取压力分别为80℃和13.1 MPa,固相萃取过程以HLB小柱为萃取柱,采用液相色谱-串联质谱分析。方法在5种微囊藻毒素质量浓度5~100μg/L内线性良好(r0.995),回收率为76.0%~118%,相对标准偏差为1.9%~12.0%,检出限为2~3μg/kg,定量下限为8~12μg/kg。该方法已用于西太湖沉积物的检测,具有较好的方法适用性。     

TA-FTIR/MS用于硝酸铵及其混合物的热化学行为研究

为评价物料混合对危险化学品热化学行为的影响,采用热分析-红外/质谱联用技术(TA-FTIR/MS)研究硝酸铵、柠檬酸和蔗糖的混合物的热化学行为。通过对硝酸铵及其混合物的分解温度和分解过程中逸出气体的分析,发现硝酸铵、柠檬酸和蔗糖的混合物热分解温度分别降低至135℃和153℃,而硝酸铵与甲基纤维素的混合物分解温度与硝酸铵基本相同为201℃,且各混合体系的气相分解产物均有氮氧化物(NOX),H2O和CO2。结果表明,混合物受热后其中的硝酸铵首先分解为硝酸和氨气;酸性物质和还原性物质由于对硝酸的分解反应有催化作用,使得混合物的热稳定性下降。     

海水中有机污染物的气相色谱－质谱法鉴定

本文采用一种简便的连续萃取装置．对海水中痕量有机物进行富集,大量的海水被萃取后,萃取物经干燥浓缩在毛细管气相色谱上进行了分离,并用质谱－计算机自动检索装置进行了定性鉴定,共确定出３６种组分。本方法的检测限为辛烷１０ｐｐｔ。