超高效液相色谱-串联质谱同步检测艾比湖中14种抗生素

采用超高效液相色谱-串联质谱法(UPLC-MS/MS),建立了同时检测水样中三类共计14种抗生素的分析方法。水样经HLB小柱萃取富集后,用10%甲醇含0.1%的甲酸溶液定容,以高效液相色谱-串联质谱对目标物进行分析。在最优实验条件下,14种抗生素的线性范围为1.0~500μg/L,相关系数均大于0.99,方法的检出限为0.30~1.23 ng/L。将建立的方法应用于检测艾比湖湖水中14种抗生素的残留分析,结果表明:14种抗生素中共检测出12种,其中氧氟沙星、洛美沙星、环丙沙星、土霉素的检出率为100%,洛美沙星的浓度最高。     

Significance of organic matter in Eocene turbidite sediments (SE Pyrenees,Spain)

Although turbidite deposits are classically considered to be good reservoir rocks for oil and gas, there are no reports concerning their source rock potential in the literature. The sediments from the Vallfogona Formation in the South-Eastern Pyrenees present numerous organic matter-rich levels interbedded in sandstones and coarse turbidite deposits. Two types of organic matter deposits were differentiated on the basis of organic geochemistry and petrography: type A and type B. Type A was deposited in a carbonate marine environment under hypersaline conditions as indicated mainly by even/odd n-alkane predominance, pristane and phytane ratio (Pr/Ph) < 1, presence of gammacerane, and trisnorneohopane over trisnorhopane ratio (Ts/Tm) > 1. Type B was deposited in a more mud-rich marine environment evidenced by the predominance of odd n-alkane, Pr/Ph ≥ 1, Ts/Tm < 1, the absence of gammacerane, similar concentrations of the C₂₇ and C₂₉ regular steranes, and the greater abundance of C₂₇ diasteranes. Turbidite facies can be regarded as an environment where organic matter sedimentation is heterogeneous in type and amount. This study suggests that turbidite deposits with interbedded organic matter-rich levels may act as a combined source–reservoir system.     

超声萃取GC/MS法测定电子电气产品中12种邻苯二甲酸酯的含量

建立了超声萃取GC/MS法测定电子电气产品中12种邻苯二甲酸酯类增塑剂的方法。结果表明:该方法简单快速,灵敏度高,相对标准偏差小于10%,加标回收率为86%~109%;样品处理过程中采用化学毒性小的乙酸乙酯作为萃取溶剂,绿色环保。经过对多批次的各种电子电气产品中12种邻苯二甲酸酯分析测定,均得到满意结果。     

超高效液相色谱-质谱联用法同时测定地下水中23种药物残留

建立了一种采用固相萃取、超高效液相色谱-质普联用技术快速并同时测定地下水中23种药物残留的方法.样品经HLB固相萃取富集净化,以反相C18柱为分离柱,甲醇和0.1%的甲酸溶液进行梯度洗脱,结合多时间段多反应监测的质谱扫描方法(mp MRM),可在10 min内同时检测地下水中10种磺胺类药物、7种喹诺酮类药物及6种β-受体激动剂药物.结果发现,该方法在1.0~100.0 ng·m L-1的浓度范围内峰面积与药物浓度呈良好的线性关系,相关系数均大于0.99,回收率在80%~110%,检测限和定量限分别为0.5 ng·m L-1和1.0 ng·m L-1.研究表明,该方法快速灵敏,专属性好,可用于地下水中药物残留的快速检测.     

蔬菜中喹诺酮类抗生素污染探查与风险评价:以广州市超市蔬菜为例

基于超声提取-固相萃取(MW-SPE)预处理方法和高效液相色谱-串联质谱(HPLC-MS/MS)分析技术,对广州市超市蔬菜中4种喹诺酮类抗生素(QNs)的污染状况进行探查与健康风险评价.结果表明,4种喹诺酮类化合物的检出率均大于90%,蔬菜(干重,下同)中单个化合物最高含量约150μg/kg,总含量(∑QNs)在10....     

活性污泥法处理焦化废水COD不达标原因分析

采用GC/MS对国内某焦化厂的主要工艺废水及生化外排水中的有机污染物进行了系统检测,分析了各主要工艺废水及生化外排水中有机污染物的组成。结果表明,造成外排水COD不达标的主要原因是由于废水中含有难降解的含氮杂环类和多环芳烃类有机物。这两类有机物主要来自焦油和苯回收精制工艺过程中产生的废水,占生化外排水中所有有机物提供的总COD的72.64%。若对这几种废水进行单独处理则可保证生化外排废水COD达标。     

硅胶管采样—气相色谱测定环境空气中苯胺类化合物

研究并建立了环境空气中7种苯胺类化合物经硅胶管吸附、甲醇解吸、气相色谱氮磷检测器检测方法。研究结果显示：当采集10 L气体时,该方法检出限为0.0059-0.0129 mg/m^3（进样量为1.0μl时）。采集样品密闭、低温可保存3 d。该方法可有效提高检出限、精密度,回收率均满足环境监测要求。     

三峡库区城市给水厂多环芳烃分布变化评价

多环芳烃PAHs(Polycyclic Aromatic Hydrocarbons)是广泛存在的典型持久性有机污染物,了解三峡库区城市供水中PAHs的分布和变化具有重要的理论和现实意义.本文选用EPA推荐的3510c液-液萃取前处理方法和GC/MS 8270c测定方法,对三峡库区6个城市自来水厂(重庆主城3个,库区3个)原水与出厂水的多环芳烃物质的种类和含量进行了测定,并对主城某水厂两套常规处理工艺各工段PAHs的分布和水平进行了分析评价.结果表明,6个水厂的原水和出厂水中检出了萘、菲、蒽、芘、荧蒽、二氢苊共6种PAHs,其中萘、蒽、荧蒽检出率较高,枯水期含量水平在1～40 ng/L.PAHs经2种常规的水处理工艺后,浓度有所降低.但滤后水经加氯消毒等工序后,PAHs浓度有所增加.     

Formation of multiple trimethylsilyl derivatives in the derivatization of 17α-ethinylestradiol with BSTFA or MSTFA followed by gas chromatography-mass spectrometry determination

N,O-bis（trimethylsily）trifluoroacetamide （BSTFA） and N-methyl-N（trimethylsily） trifluoroacetamide （MSTFA） are common derivatization reagents used in the GC-MS analysis of estrogen steroids such as estrone （El） and 17α-ethinylestradiol （EE2）. In this study, three trimethylsilyl （TMS） steroid derivatives, mono- and di-trimethylsilyl EE2 and mono-trimethylsilyl El, were observed during the derivatization of EE2 with BSTFA or MSTFA and/or GC separation. Factors influencing the production of multiple TMS derivatives and their relative abundance were examined. It was found that both methanol and bisphenol A competed with estrogenic esteroids when reacting with silylation reagents, and thus affected the formation of TMS derivatives and their relative abundance in the derivatization products. Methanol was found to be more reactive than bisphenol A with the BSTFA reagent. None of the three solvents tested in this study could prevent the generation of multiple TMS derivatives during the derivatization of EE2 with BSTFA, followed by GC analysis. A similar result was observed using MSTFA as the derivative reagent followed by GC analysis. Thus, the suitability of BSTFA or MSTFA as the derivatization reagent for the determination of E1 and EE2 by GC-MS, under the conditions reported here, is questionable. This problem can be solved by adding trimethylsilylimidaz （TMSI） in the BSTFA reagent as recommended, and the performance of the method has been proved in this study.     

大气中痕量烯烃的观测与分析

采用两步深冷冻浓缩自动进样系统,配以气相色谱/质谱联机对北京大气中的烯烃进行了连续观测.结果表明,北京市大气中浓度最高的烯烃为C4烯烃,2000年日平均浓度为3.5×10^-9±3.0×10^-9(V/V).2h平均浓度的日变化在春、夏、秋、冬4季各有特点,但基本上呈双峰型模态,峰值分别出现在上午和傍晚;在季节变化中,1、10月份大气中C4烯烃的浓度最高,为6.0×10-9±1.2×10^-9(V/V),3、9月份最低,为0.31×10^-9±0.13×10^-9(V/V).