高效液相色谱串联质谱法分析土壤中多溴联苯醚类化合物

建立了一种超高效液相色谱串联质谱法(UPLC-MS/MS)同时测定土壤中8种多溴联苯醚化合物(PBDEs)的方法,采用快速溶剂萃取(ASE)和凝胶净化色谱(GPC),经BEH反相C₁₈色谱柱分离,10 min内完成分离,使用含0.1%氨水的甲醇和水进行梯度洗脱,采用液相色谱-负离子-大气压化学电离(APCI)串联质谱,多反应监测模式(MRM),加入 ¹³C₁₂-BDE-139和¹³C₁₂-BDE-209内标作定量分析。结果表明:在优化的分析条件下,PBDEs的线性相关系数为0.998 8～0.999 5,方法检出限为0.22～0.59 μg/kg,在2个添加水平下,平均回收率为71%～126%,标准偏差为3%～18%,土壤实际质控样测定结果均在允许范围内。适合于土壤中PBDEs的快速分析,特别对于高溴代PBDEs,相比气相色谱质谱方法具有更快的分析速度和更好的稳定性。     

固相萃取-高效液相色谱-质谱联用法用于地表水中类固醇激素测定

建立了固相萃取-高效液相色谱-质谱联用法对雌三醇、氟哌噻吨、炔雌醇、雄烯二酮、雌二醇、雌酚酮、睾酮共7种类固醇激素的检测方法。样品经C18萃取小柱富集净化,采用内标法定量时,方法的检出限为0.66～1.95 ng/L,R0.998,回收率为78.5%～94.6%,相对标准偏差为1.1%～7.7%。采用该方法对上海市地表水进行测定,在2个采样点中检出雌酚酮(1.88 ng/L)和雄烯二酮(1.48 ng/L)。     

土壤中挥发性有机物的快速测定方法

本文建立了用便携式气相色谱-质谱仪快速测定土壤中VOCs的方法。该方法能够快速对土壤样品中VOCs进行定性分析和定量测定。当采样量达到5 g时,方法检出限0.02~2.11μg/L,相对标准偏差2.0%~13.5%;加标20μg/L时,回收率63%~123%。采用该方法测定北京地区5个土壤样品,总体质量浓度为0~873μg/kg。     

Biogas from the organic fraction of municipal solid waste: Dealing with contaminants for a solid oxide fuel cell energy generator

The present work investigates electricity production using a high efficiency electrochemical generator that employs as fuel a biogas from the dry anaerobic digestion of the organic fraction of municipal solid waste (OFMSW).The as-produced biogas contains several contaminants (sulfur, halogen, organic silicon and aromatic compounds) that can be harmful for the fuel cell: these were monitored via an innovative mass spectrometry technique that enables for in-line and real-time quantification.A cleaning trap with activated carbons for the removal of sulfur and other VOCs contained in the biogas was also tested and monitored by observing the different breakthrough times of studied contaminants.The electrochemical generator was a commercial Ni anode-supported planar Solid Oxide Fuel Cell (SOFC), tested for more than 300 h with a simulated biogas mixture (CH₄ 60 vol.%, CO₂ 40 vol.%), directly fed to the anode electrode. Air was added to promote the direct internal conversion of CH₄ to H₂ and CO via partial oxidation (POx).The initial breakthrough of H₂S from the cleaning section was also simulated and tested by adding ～1 ppm(v) of sulfur in the anode feed; a full recovery of the fuel cell performance after 24 h of sulfur exposure (～1 ppm(v)) was observed upon its removal, indicating the reliable time of anode exposure to sulfur in case of exhausted guard bed.     

Anaerobic co-digestion of food waste and landfill leachate in single-phase batch reactors

In order to investigate the effect of raw leachate on anaerobic digestion of food waste, co-digestions of food waste with raw leachate were carried out. A series of single-phase batch mesophilic (35 ± 1 °C) anaerobic digestions were performed at a food waste concentration of 41.8 g VS/L. The results showed that inhibition of biogas production by volatile fatty acids (VFA) occurred without raw leachate addition. A certain amount of raw leachate in the reactors effectively relieved acidic inhibition caused by VFA accumulation, and the system maintained stable with methane yield of 369–466 mL/g VS. Total ammonia nitrogen introduced into the digestion systems with initial 2000–3000 mgNH₄–N/L not only replenished nitrogen for bacterial growth, but also formed a buffer system with VFA to maintain a delicate biochemical balance between the acidogenic and methanogenic microorganisms. UV spectroscopy and fluorescence excitation–emission matrix spectroscopy data showed that food waste was completely degraded.We concluded that using raw leachate for supplement water addition and pH modifier on anaerobic digestion of food waste was effective. An appropriate fraction of leachate could stimulate methanogenic activity and enhance biogas production.     

移动床生物膜反应器用于苯酚废水处理的性能研究

实验应用移动床生物膜反应器处理人工配制的苯酚废水,研究了在不同的苯酚进水浓度和不同的水力停留时间时苯酚的去除效率,以及反应器对冲击负荷的承受能力.结果表明,在水力停留时间为24 h、苯酚进水浓度从200 mg·L-逐渐上升至1400 mg·L-1以及苯酚进水浓度1000 mg·L-1、水力停留时间从32 h逐渐降至16 h的条件下,苯酚均能够被完全去除.对冲击负荷,MBBR具有较强的承受能力.由荧光原位杂交技术分析可知,酵母菌和真细菌是反应器中降解苯酚的主要微生物.说明移动床生物膜工艺能够高效地用于苯酚废水处理之中.     

石墨炉原子吸收分光光度法测定土壤中总铬

建立了土壤中总铬测定的石墨炉原子吸收分光光度法;以塞曼效应扣除背景,优化了石墨炉灰化、原子化温度、停留时间及基体改进剂用量。结果表明:当原子化温度为2 700℃,灰化温度为700℃,原子化时间2 s,灰化时间为9 s;基体改进剂用量为3~5μL时,仪器可以达到最佳工作状态。该方法铬元素浓度在0~32μg/L内呈良好的线性关系,相关系数r=0.999 9,检出限为0.3 mg/kg;对土壤标样GSS-1和ESS-1的铬测定精密度均小于5%,相对误差在-4.8%~-0.7%之间,方法的灵敏度和准确度均符合要求。因此,石墨炉原子吸收分光光度法测定土壤中总铬具有原子化温度高、干扰少、灵敏度高等特点可适用土壤中总铬的测定。     

水质沙门氏菌群的MUCAP试验初步研究

利用沙门氏菌分解底物形万物地征性荧光的特性，建立了水质沙门氏菌群的”酶－底物“快速检测方法。检测试剂由上医大实验室自行合成，经红外，质谱，核磁共振分析，证明其结构与国报道一致，纯度可达９９．９９％。ＭＵＣＡＰ试验的反应参数；底物最家度为３７．５μｇ／ｍｌ，反应最适ＰＨ为７．２－７．４。细菌密度和荧光强度随着培养时间增加而增加，敏感度为１０＾６只／ｍｌ，该检测法有较高特异，水中常见的１０种细菌未有明     

Prenatal identification of a 45,X/46,Xder(Y) mosaicism and confirmation by high resolution cytogenetics and fluorescence in situ hybridization

A 45,X/46,Xder(Y) mosaicism detected prenatally was shown to have a rare Y inversion- duplication or Y/Y translocation which can only be identified by a combination of high resolution cytogenetics and fluorescence in situ hybridization. The present data indicate the usefulness and importance of chromosome-specific probes in the identification and characterization of chromosome rearrangements.     

石墨炉原子吸收法测定土壤中微量钒

以石墨炉原子吸收法测定土壤中微量钒。选择了最佳仪器测定条件和样品消解条件。方法的最低检出浓度为0.030mg/l,变异系数为4.7％。