基于直接进样-超高效液相色谱串联质谱法的水中2甲4氯残留测定

针对目前水体中MCPA检测灵敏度不够,缺乏一种无需前处理、可直接上机、简单便捷方法的问题,以超高液相色谱串联质谱仪,建立了一种以电喷雾离子源ESI-为电离模式、MRM为监测模式、可直接进样测定水体中MCPA残留的方法。结果表明,最优方法条件为定量离子对199.0/140.9(m/z),流动相乙腈和水梯度洗脱,色谱柱Acquity UPLC HSS T3。在MCPA质量浓度为0.1~100μg/L范围内线性良好(R2=99.99%),检出限为0.006μg/L,定量限为0.018μg/L,是现有直接进样法的23~83倍,完全满足水体中MCPA的检测要求(<0.1μg/L)。在添加水平为1~100μg/L时,回收率为94.30%~105.60%,相对标准偏差为1.05%~3.61%,具有前处理简单、准确性高、精密度好、灵敏度高等优点。     

HPLC/MSn法鉴定环境激素邻苯二甲酸丁基苄酯在小鼠尿中的代谢产物

应用HPLC-MSⁿ方法,研究了邻苯二甲酸丁基苄酯在小鼠尿液中的代谢产物,并对尿中推测的代谢物和标准品分别进行HPLC-UV和二级全扫描质谱（MS²）分析,结果在尿中发现了6个代谢产物,分别为邻苯二甲酸、马脲酸、邻苯二甲酸单丁酯、邻苯二甲酸苄酯、邻苯二甲酸单丁酯葡萄糖醛酸结合物及邻苯二甲酸苄酯葡萄糖醛酸结合物.推断环境激素邻苯二甲酸丁基苄酯在小鼠体内的代谢途径为原形首先水解生成邻苯二甲酸单丁酯、邻苯二甲酸苄酯、邻苯二甲酸,部分邻苯二甲酸发生脱羧反应生成苯甲酸,苯甲酸再与内源性物质甘氨酸结合成马脲酸,邻苯二甲酸单丁酯、邻苯二甲酸苄酯和内源性β-D-葡萄糖醛酸结合,生成水溶性较大的邻苯二甲酸单丁酯葡萄糖醛酸结合物和邻苯二甲酸苄酯葡萄糖醛酸结合物.     

气质谱联用仪在环境监测中的应用

气相色谱一质谱联用仪（GC-MS）因其准确、快速、高灵敏度等优点在环境监测中被广泛应用。文章介绍了GC-MS仪仪器类型,综述了其在水环境,大气环境,恶臭物质方面的应用研究。     

吹扫捕集—气相色谱／质谱联用测定饮用水中59种挥发性有机物

建立了吹扫捕集一气相色谱／质谱联用测定饮用水中59种挥发性有机物的方法,方法检出限为0．004～0．085μg/L,可满足饮用水中特定有机分析项目的检测要求。     

长期施用粪肥菜地土壤中四环素类抗生素的含量与分布特征

规模化养殖场动物粪肥富含抗生素且作为有机肥大量施用于农业生产,由此造成的土壤抗生素污染问题在我国还鲜有研究.针对亚热带地区长期施用粪肥的“无公害蔬菜”生产基地,利用固相萃取-高效液相色谱-串联质谱(HPLC-MS/MS)分析方法,探讨了土壤中4种四环素类(TCs)化合物(四环素、土霉素、金霉素、强力霉素)的含量与分布特征.结果表明,土壤中4种四环素类化合物的总含量(TCs)在1.35～22.52 μg/kg之间,平均为7.35 μg/kg.各化合物的检出率在31%～100%之间,平均含量为0.63～3.11 μg/kg,以土霉素和强力霉素为主.化合物的含量与组成特征无论在平面上还是在剖面上均存在明显的空间分布差异,且随着深度增加含量迅速降低,但在80 cm深度仍有检出.土壤中四环素类化合物的含量较低,生态毒性风险较小,但化合物的检出率较高且普遍同时检出多种化合物,其协同生态毒性尤其是耐药性问题值得进一步研究.     

高效液相色谱质谱法测定地表水中丙烯酰胺

文章探索了高效液相色谱质谱法检测丙烯酰胺的方法:将水样直接进样,用高效液相色谱质谱仪测定,其检出限为0.1μg/L,方法回收率在93.6%~112%,相对标准偏差范围2.3%~7.9%。完全满足世界卫生组织、《生活饮用水标准》和《地表水环境质量标准》设定的丙烯酰胺限量0.5μg/L的要求。且此方法前处理操作简单,结果准确可靠。     

气氛对快速催化热解生物质的影响

通过测定两种气氛下(氮气和二氧化碳)的催化热解(HZSM-5为催化剂)的产率,并利用气质联用仪(GC/MS)分析热解油的成分,研究这两种热解气氛对快速催化热解生物质(玉米杆)的产率和液体产物的影响差异。结果表明:改变热解气氛对结果产生明显影响,CO2气氛对催化热解不利,该气氛下的固液气产率分别为30.30%,37.89%,31.81%,CO2促使快速催化热解的液体产量降低,促进水相产物的生成。对催化热解油的分析发现CO2气氛抑制了HZSM-5的去氧和芳香化催化作用,同时促进稠环芳烃的生成,使产物结构复杂化。     

The inactivation of bacteriophages MS2 and PhiX174 by nanoscale zero-valent iron: Resistance difference and mechanisms

• The resistance of phage PhiX174 to nZVI was much stronger than that of MS2. • The nZVI damaged the surface proteins of both bacteriophages. • The nZVI could destroy the nucleic acid of MS2, but not that of PhiX174. •The phage inactivation was mainly attributed to the damage of the nucleic acid. Pathogenic enteric viruses pose a significant risk to human health. Nanoscale zero-valent iron (nZVI), a novel material for environmental remediation, has been shown to be a promising tool for disinfection. However, the existing research has typically utilized MS2 or f2 bacteriophages to investigate the antimicrobial properties of nZVI, and the resistance difference between bacteriophages, which is important for the application of disinfection technologies, is not yet understood. Here, MS2 and PhiX174 containing RNA and DNA, respectively, were used as model viruses to investigate the resistances to nZVI. The bacteriophage inactivation mechanisms were also discussed using TEM images, protein, and nucleic acid analysis. The results showed that an initial concentration of 10⁶ PFU/mL of MS2 could be completely inactivated within 240 min by 40 mg/L nZVI at pH 7, whereas the complete inactivation of PhiX174 could not be achieved by extending the reaction time, increasing the nZVI dosage, or changing the dosing means. This indicates that the resistance of phage PhiX174 to nZVI was much stronger than that of MS2. TEM images indicated that the viral particle shape was distorted, and the capsid shell was ruptured by nZVI. The damage to viral surface proteins in both phages was examined by three-dimensional fluorescence spectrum and sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE). However, the nucleic acid analysis demonstrated that the nucleic acid of MS2, but not PhiX174, was destroyed. It indicated that bacteriophage inactivation was mainly attributed to the damage of nucleic acids.     

人体呼出气中内源性挥发性有机物筛选研究

人体代谢产生的内源性挥发性有机物（VOCs）可用作健康状况的标志物.本研究选择17~26岁无呼吸系统疾病的高校学生（73人）作为观察对象,使用气相色谱-火焰离子化检测器/质谱联用仪（GC-FID/MS）分析收集到的呼出气样本,对呼出气中VOCs的种类、浓度进行研究,发现了其5种卤代物的浓度高于室内浓度,其次是室外浓度.其中,在人体呼出气中1,1-二氯乙烯的浓度为室内浓度的近20倍,是室外浓度的近300倍,人体呼出气是环境中1,1-二氯乙烯的一个重要源.定量分析健康人呼出气,对比其与环境空气样本的浓度差异,并进行统计学检验,共筛选出1,1二氯乙烯、丙酮、1-己烯、甲基环己烷、2-戊酮、反-2-戊烯、2,4-二甲基戊烷、3-戊酮、四氯乙烯、对二氯苯、间二氯苯11种特征性内源性VOCs.     

Organic pollutants in snow of urban and rural Russia and Finland

To check the effect of possible deposition of organic contaminants in northern regions of the Earth due to atmospheric transport snow samples were collected in early March in 6 places in Russia and 4 in Finland including arctic territories. GC‐MS was used as an analytical tool to identify and quantify individual organic compounds belonging to the various classes. As a result more than 250 compounds were detected. The possible presence of more than 100 other priority pollutants from the US EPA list was also screened.