高效液相色谱-串联质谱法同时检测地表水中13种药物及个人护理品

采用高效液相色谱-串联质谱(HPLC-MS/MS)检测,建立了地表水中13种药物及个人护理品的测定方法。水样用盐酸与氢氧化钠溶液调p H值至7.0左右,过固相萃取小柱进行富集,用14 m L甲醇洗脱。以C18柱为分离柱,0.01%甲酸的甲醇-0.01%甲酸水溶液为流动相,目标物在10 min内分离,在0.50~250μg/L范围内,13种化合物峰面积与内标物质峰面积之比与质量浓度的线性关系良好(0.99),检出限在0.05~0.5 ng/L范围内。基质加标实验结果表明,13种化合物在水中的回收率分别在56.2%~123.2%之间(加标水平5 ng/m L)和58.0%~107.8%(加标水平50 ng/m L),相对标准偏差在1.60%~19.9%(n=6)之间。应用该方法测定了从2条纳污河流采集的10份水样,结果表明,除美托诺尔和普洛萘尔未被检出外,其余11药物的检出频率在30%~100%之间。在13种目标物质中,咖啡因的检测浓度最高达287.5ng/L,舒必利次之,为277.5 ng/L。本方法快速、准确,适用于地表水中PPCPs类的快速测定。     

流动注射-氢化物发生-原子荧光光谱法测定土壤中铅

采用流动注射-氢化物发生-原子荧光光谱法测定土壤中的铅,工作曲线线性关系良好,检出限为0.25 mg/kg,相对标准偏差＜3.5%,加标回收率为93.0%～105%.该方法简便快速,测定结果准确可靠.     

长江河口硅和磷生源要素质量浓度的变化特征

根据近年来长江河口区域内大通水文站的记录和近期在长江入海河口区上海段多个采样点的生源要素质量浓度实测数据,比较水中可溶性硅酸盐和磷酸盐的质量浓度,分析在长江入海河口区水中硅和磷元素含量的主要变化特征.结果表明,长江水中的硅酸盐和磷酸盐从长江入海河口进入大海的过程中,其质量浓度有降低的趋势,它们在长江入海河口的多年的质量浓度变化趋势是相反的.长江入海河口区域上游的磷酸盐质量浓度升高幅度较大,而硅酸盐变化不大,硅酸盐、磷酸盐质量浓度在长江河口区进入海洋的过程中迅速降低.      

Mass transport model of ions within biofilms under the effect of external field

A mass transport model was developed to predict the transport rate of ions within biofilms, which was experimentally verified using the fluxes of NH4^＋ and Ca^2＋ through the heterotrophic biofilms with the thickness varying from 230 to 1430μm under the effect of external field in the range of-20 V/m to 60 V/m. It is found that the result predicted by the model is in agreement with the experimentally obtained one, with the error less than 5 percent for the thin biofilms. The error increases with the increase of the biofilm thickness. The transport rate of ions caused by electric migration is affected by the charges, field strength, and biofilm thickness and so on.     

典型软垫家具材料火灾特性的小尺寸实验研究

本文借助锥型量热计对制作软垫家具的材料进行小尺寸实验,获得了典型软垫家具面料、聚氨酯海绵填料及其组合件的燃烧性能参数。通过对实验获得参数的分析比较,认为面料对组合件燃烧特性的影响大,仅使用阻燃布就可以明显改善组合的火灾特性。     

基于RFPA2D复合局部挠曲岩体数值模拟

为研究复合局部挠曲岩体强度特征以及破坏规律,采用岩石真实破裂软件RFPA^2D,对水平层面挠曲30°,45°,60°,75°的复合岩体进行单轴压缩试验模拟。模拟结果表明:挠曲角为30°,45°,60°,75°的复合岩体破坏面几乎与挠曲段夹层重合,其挠曲端部均产生了垂直于挠曲段夹层的裂纹;复合单斜岩体与复合挠曲岩体破坏面的形成因素大致相同,夹层强度是2种岩体失稳的主要因素;复合挠曲岩体单轴抗压强度随挠曲角增大同样呈“U”型变化,与单斜岩体变化趋势一致;当水平层状岩体发生挠曲后,其单轴抗压强度减小,当挠曲角为60°时,强度降低25.19%,当挠曲角为75°时,强度降低0.17%。;随着均质系数m的增大,复合挠曲岩体单轴抗压强度以及轴向应变均出现逐渐递增的趋势,且不同m值,其岩体裂隙扩展方式具有明显差别。     

高效液相色谱-三重四级杆/复合线性离子阱质谱法测定饮用水中22种邻苯二甲酸酯

建立了一种同时测定饮用水中22种邻苯二甲酸酯(PAEs)的高效液相色谱-三重四级杆/复合线性离子阱质谱方法:饮用水样品经针头过滤器过滤,选用Biphenyl液相色谱柱进行分离,以含0.1%甲酸的水溶液和含0.1%甲酸的甲醇溶液为流动相,电离模式为电喷雾正离子,选用多反应监测触发增强子离子扫描模式进行检测。结果表明,22种PAEs的灵敏度良好,定量限为0.001～0.1 μg/L。配制浓度为0.1～100.0 μg/L的混标溶液进行进样分析,分析结果显示,22种PAEs在该范围内的线性关系良好,相关系数均大于0.995,方法的平均回收率为82.9%～108.9%,相对标准偏差为0.9%～11.2%。同时,使用增强子离子扫描谱图进行搜库匹配,定性准确性高。该方法适用于饮用水中PAEs的检测。     

液氮泡沫发生器内流动特性研究

低温液氮与泡沫混合液直接接触产生氮气泡沫是一种新型的掺混形式,利用液氮高汽化比的特点,搭建液氮泡沫可视化实验装置,进行氮气-水两相流及液氮泡沫流动特性的研究。结果表明,液氮相变产生大量氮气,其与泡沫液混合产生泡沫,温度有所回升,最终趋于泡沫混合液温度;管路沿程压降较小;液氮射流破碎及流动过程可分为6个区域:低温液氮区、向上循环翻滚区、滞留区、泡沫与泡沫混合液混合区、致密泡沫区、泡沫混合液区。流体向下游流动过程中持续发泡;为防止管路结冰,需合理控制泡沫混合液与液氮流量。     

An LC-MS/MS method for creatine and creatinine analysis in paraquat-intoxicated patients

Abstract

A sudden increase in serum creatinine after paraquat intoxication has been reported in several clinical studies. However, this dramatic change of creatinine may be possibly due to an interconversion of creatine-creatinine in relation to paraquat toxicity. In order to investigate the creatine-creatinine relationship, a liquid chromatography tandem mass spectrometry in combination with electrospray ionization was developed and validated for simultaneous determination of creatine and creatinine in the serum. The chromatographic separation was achieved on a Gemini® C₆-Phenyl column with a gradient elution consisting of 0.1% formic acid in ultrapure water and methanol as the mobile phase. The method yielded suitable levels of specificity and selectivity, and calibration curves of creatine and creatinine in serum were linear over the concentration range of 0.5–200?µg mL^?1. The limit of quantification of both compounds was 0.5?µg mL^?1, and the method was accurate within the recovery range of 96.23–102.75%, indicating the robustness of the method. The method was successfully applied to toxicological samples from paraquat-intoxicated patients, and the concentrations of creatine and creatinine were quantified. High creatine concentrations in serum samples were observed which may lead to high serum creatinine despite normal kidney function as creatine is converted to creatinine in proportion to its concentration.     

气相色谱-串联质谱法测定沉积物中多环芳烃

采用ASE法提取沉积物中16种多环芳烃,以固相萃取法净化提取液,用气相色谱-串联质谱法测定。通过优化测定条件,使方法在5.00μg/L~1 600μg/L范围内线性良好,方法检出限为0.15μg/kg~0.66μg/kg。空白石英砂的加标回收率为61.9%~121%,7次测定结果的RSD为2.6%~11.1%。