水环境中26种类固醇激素的分析方法研究

建立了固相萃取-超高效液相-串联质谱法同时测定水环境中26种类固醇激素的分析方法。明确了取样体积为500 m L,Cleanert PEP为富集柱,乙酸乙酯为洗脱剂,甲醇为溶剂进行提取操作。选择了正离子模式,以0. 1%甲酸/甲醇-水为流动相,负离子模式以0. 1%氨水/乙腈-水为流动相,试样经AcquityTMUPLC BEH C18色谱柱分离后,选用质谱检测模式进行定性、定量分析。通过方法验证,26种类固醇激素的方法检出限为0. 3～1. 5 ng/L,测定下限为1. 2～6. 0 ng/L,代表性样品测定结果的相对标准偏差为2. 6%～13. 7%(n=6),加标回收率为71. 2%～121%。该方法操作便捷,灵敏度高,精密度和准确度良好,可适用于水环境中多种痕量、超痕量类固醇激素的定性定量分析。     

气相色谱-质谱法测定废酸油渣中的16种多环芳烃

建立了废酸油渣中16种多环芳烃超声萃取、Florisil萃取柱净化、气相色谱-质谱测定的方法.笔者对提取方式、提取剂类型和体积、提取时间和次数、净化方式等进行研究,采用无水硫酸钠分散,二氯甲烷作为提取剂超声40 min,提取液经纯水清洗、离心后取适量有机相经过3 g Florisil萃取柱净化,采用气相色谱-质谱选择离...     

混合酸消解变化对土壤和沉积物中痕量硒分析影响

基于各3种采集环境样本、国家标准物质的土壤和沉积物,以当前环境监测行业常用的3种消解方法,探讨20种混合酸系统条件在消解条件变化中对复杂样本硒元素测定的影响.确定了最佳土壤和沉积物消解的组合为王水系统(盐酸∶硝酸∶氢氟酸∶过氧化氢∶高氯酸=3∶1∶1∶1∶1),各消解法的处理结果部分(n=5):水浴法消解时间仅需0.5...     

地表水中微量氯代芳烃和硝基取代芳烃化合物的分析方法

建立了固相萃取、毛细管气相色谱-电子捕获检测、内标标准曲线法定量分析地表水中十三种氯苯、硝基氯苯和硝基苯类化合物的方法.该法对这些化合物的平均回收率在62%-101%之间,变异系数在3%-27%之间,方法最小检测浓度在0.01-1.31μg·1-1之间.应用本方法对太湖水中的氯代芳烃和硝基取代芳烃化合物进行了三次采样分析,定量重现性较好.     

云南高原典型林分林下枯落物持水特征研究

森林枯落物具有重要生态水文功能,通过实地调查与实验分析,对云南高原湖泊纳帕海流域3种典型林分枯落物储量、持水量和持水过程进行了研究。结果表明：高山松（pinus densata）林下枯落物储量最大,白桦林（Betula platyphylla Suk.）次之,川滇高山栎（Quercus aquifolioides）灌丛最小,林下枯落物储量最大持水量和有效拦蓄量大小排序表现出和枯落物储量相同的顺序;不论是储量、最大持水量还是有效拦蓄量,各林分枯落物都表现出半分层大于未分解层。3种林下枯落物在0～2 h内吸水较快,在10 h后吸水速明显减缓,用对数方程对3种林下枯落物未分解层和半分解层持水量与浸水时间进行拟合,用幂函数方程对吸水速率与浸水时间进行拟合,结果显示相关系数都较高。     

Cd胁迫下As污染土壤对农作物生长及农产品安全性的影响

采用盆栽实验的方法研究了在Cd胁迫下As污染物对水稻(Oryze sativa L.)、大豆(Glycine mdx L .)生长发育及重金属吸收积累的影响,As-Cd污染土壤采用不同改性剂对农产品安全性的影响研究.研究结果表明:单元素As处理与对照相比水稻株高降低了10.3锄、产量下降了9.8%,而大豆株高、产量分别增加了6 cm、36.9%,在实验设计污染物浓度范围内,As对大豆生长发育有刺激作用.As-Cd处理与对照相比水稻的株高、产量分别下降了2.3 cm、1.75%,而大豆株高、产量下降了12 cm、5.6%,As-Cd污染处理抑制了作物的生长发育;As-Cd处理比单元素As处理其水稻籽实、茎叶、根中As含量分别多4.2倍、1.14倍、1.7倍,As-Cd处理比单元素As处理大豆籽实、茎叶、根中As含量分别多4.63倍、2.82倍、1.85倍,Cd元素的存在对水稻、大豆吸收As具有协同作用;采用腐殖酸4%、pH4处理改性措施使土壤中有效态As含量降低,降低了As对农作物的健康风险.     

Discovery of emerging organic pollutants in the atmosphere through an omics approach

● We review the framework of discovering emerging pollutants through an omics approach. ● High-resolution MS can digitalize atmospheric samples to full-component data. ● Chemical features and databases can help to translate untargeted data to compounds. ● Biological effect-directed untargeted analyses consider both existence and toxicity. Ambient air pollution, containing numerous known and hitherto unknown compounds, is a major risk factor for public health. The discovery of harmful components is the prerequisite for pollution control; however, this raises a great challenge on recognizing previously unknown species. Here we systematically review the analytical techniques on air pollution in the framework of an omics approach, with a brief introduction on sample preparation and analysis, and in more detail, compounds prioritization and identification. Through high-resolution mass spectrometry (HRMS, typically coupled with chromatography), the complicated environmental matrix can be digitalized into “full-component” data. A key step to discover emerging compounds is the prioritization of compounds from massive data. Chemical fingerprints, suspect lists and biological effects are the most vital untargeted strategies for comprehensively screening critical and hazardous substances. Afterward, compressed data of compounds can be identified at various confidence levels according to exact mass and the derived molecular formula, MS libraries, and authentic standards. Such an omics approach on full-component data provides a paradigm for discovering emerging air pollutants; nonetheless, new technological advancements of instruments and databases are warranted for further tracking the environmental behaviors, hence to evaluate the health risk of key pollutants.     

LC-MS/MS determination of pesticide residues in fruits and vegetables

The aim of the research is to evaluate pesticide residue contamination of fresh and frozen fruits and vegetables, agricultural raw material, purchased from Polish farmers for production of frozen fruits and vegetables, and the estimation of the multiresidue method effectiveness expressed as the proportion of pesticides detected in food samples to the total number of pesticides analyzed by multiresidue methods. A total of 144 samples (of black currants, red currants, raspberries, cherries, strawberries, blackberries, cauliflowers and broccoli) were analyzed using LC-MS/MS method for the determination of 60 pesticides. QuEChERS extraction, matrix-matched calibration and dynamic multiple reaction monitoring method were used. Residues of 15 compounds, mainly fungicides and insecticides, were detected in 46 samples. The percentage of samples with residues above the maximum residue levels (MRL) was 15%, whereas samples with residues below MRL were 17%. A total of 13 samples contained more than one pesticide residue. Pesticide residues were detected most often in samples of black currants (50%), broccoli (36.4%), raspberries (29%) and red currants (21.8%). The most frequently detected pesticides were carbendazim and acetamiprid. The proportion of pesticides detected during our study to the total number of analyzed pesticides amounted to 25%. It was compared to literature findings. For three fourth of multiresidue methods, the proportion was below 50% for methods developed for the analysis of less than 100 pesticides, and below 30% for methods developed for the analysis of more than 100 pesticides. It appears that a lot of efforts and means is lost on pesticides never or rarely detected in examined samples. The workload and cost effectiveness of the development and application of multiresidue methods along with the range of pesticides covered by the method should be carefully and thoroughly considered anytime when a new method or workflow is developed. Including non-targeted screenings in pesticide residue control seems to be an alternative worth considering.     

气质联用分析加硫酸化污泥中的有机酸

分别采用两种前处理方法分离富集加硫酸化污泥中的有机酸.方法一,利用阴离子交换树脂分离富集有机酸,在不洗脱的情况下直接和乙醇进行酯化反应,然后进行气质联用分析;方法二,利用活性炭纤维吸附型固相微萃取(ACF-SPME)的方法,顶空萃取分离后进行气质联用分析.两种方法的分析结果都未检测到酸化污泥中存在短链的有机酸,只检测到个别长链的和带苯环结构的有机酸.