便携式气相色谱测定固定源排气中的硫化氢

在SO₂与H₂S共存下,利用便携式气相色谱法测定了固定污染源排气中硫化氢含量。方法简便快速,准确度和精密度较高,受干扰物质二氧化硫的影响小,测定结果完全满足复杂成分烟气中硫化氢的测定要求。     

自动进样及气体分流技术测定气体中非甲烷总烃

采用自动进样和气体分流技术,双柱双FID检测器气相色谱法测定气体中的非甲烷总烃,实现了非甲烷总烃的连续自动分析,同时一次进样即可得到甲烷和总烃的数据。方法的检出限为0.05 mg/m3,测定的相对标准偏差在0.7%~1.8%内,非甲烷总烃的加标回收率为96.0%~98.5%。与传统手动进样法相比,本方法具有重复性好、操...     

糠醛衍生-气相色谱/质谱法测定地表水中的肼和偏二甲基肼

建立了糠醛衍生-气相色谱/质谱法测定地表水中肼和偏二甲基肼两种肼类化合物的方法,优化了实验条件.在200mL水样(pH=7)中加入10mL0.05g/mL的糠醛衍生试剂,室温下反应2h,用15mL二氯甲烷萃取10min,氮吹至1.0mL后进样分析.本方法在0～100μg/L范围内线性良好,相关系数大于0.996.检出限...     

树舌灵芝菌丝体不皂化物GC—MS分析

在树舌灵芝菌丝体化学成分研究中,采用乙醚抽提法获取树舌灵芝菌丝体脂溶性物质,经皂化后使用气相色谱一质谱联用技术（CC—MS）进行分析,共鉴定出19种物质,所得到的丁羟甲苯、乙酰菲、5,6-二氢麦角甾醇对树舌灵芝菌丝体化学成分研究具有较高价值。     

不同功能区表层土中全氟化合物污染指纹及其来源解析

为探究区域功能对其表层土中全氟化合物(perfluorinated compounds,PFCs)污染指纹与含量水平的影响,采用固相萃取分离富集、高效液相色谱-质谱联用与源解析相结合的方法,分析了深圳市公园、居民小区、十字路口、工厂周边4个功能区和城市背景共76份表层土中14种PFCs的含量.结果表明,深圳市表层土总PFCs(ΣPFCs)含量受区域功能影响显著,呈工厂周边(P<0.001)>>十字路口(P<0.01)>>居民小区(P<0.05)>>公园>城市背景的分布.其中工厂周边、居民小区、公园表层土中PFCs呈中链(P<0.05)>>长链>短链的分布,而十字路口则呈中链≈短链(P<0.05)>>长链的分布.同时,以全氟辛烷磺酸、全氟辛酸、全氟十三酸为主要标志物的3个主成分可以解释深圳表层土超过81%的ΣPFCs,十字路口以及电镀、油漆厂周边表层土呈现出较清晰的PFCs污染指纹.     

嘉兴市地表水中兽用抗生素的污染现状调查

建立了适合长三角地区重要生猪养殖基地嘉兴市环境水体中4类(四环素类、磺胺类、大环内酯类、喹诺酮类)共10种常用兽用抗生素同时检测的固相萃取与液相色谱质谱(LC-MS/MS)联用技术,对该地区10个典型村镇河道断面和21个市区主要河网监控断面开展调查.结果表明,村镇河道中抗生素污染严重,10种抗生素总浓度为65.6～467.0 ng.L-1.其中,四环素类和磺胺类浓度分别为40.8～253.0 ng.L-1和未检出～165.0 ng.L-1;大环内酯类和喹诺酮类浓度分别为3.1～14.68ng.L-1和未检出～14.54 ng.L-1.市区河网污染相对较轻,10种抗生素总浓度为20.1～61.2 ng.L-1,其中四环素类浓度为未检出～44.0 ng.L-1;磺胺类、大环内酯类和喹诺酮类浓度则分别低于2.7、6.3和21.6 ng.L-1.     

在线固相萃取-超高效液相色谱-三重四极杆质谱快速测定地表水中磺胺类抗生素

建立了在线固相萃取-超高效液相色谱-三重四极杆质谱联用技术测定地表水中痕量磺胺类抗生素的方法。样品经滤膜过滤,HLB在线固相萃取小柱富集纯化,以Acquity BEH 130为分析柱,三重四极杆质谱进行检测,外标法定量。通过在线固相萃取,并对色谱和质谱等条件进行优化,该方法检出限为0.2~1.1 ng/L,回收率为80.6%~113%,相对标准偏差<10.6%,浓度范围内线性良好（r＞0.9972）,满足了磺胺类抗生素痕量分析测试的要求,且分析时间仅需17min。该方法灵敏度高、分析速度快,对于保障水环境安全,及时提供污染信息,有效应对环境应急突发事件具有十分重要的意义。     

Formation potential and analysis of 32 regulated and unregulated disinfection by-products: Two new simplified methods

Water disinfection is an essential process that provides safe water by inactivating pathogens that cause waterborne diseases. However, disinfectants react with organic matter naturally present in water, leading to the formation of disinfection by-products (DBPs). Multi-analyte methods based on mass spectrometry (MS) are preferred to quantify multiple DBP classes at once however, most require extensive sample pre-treatment and significant resources. In this study, two analytical methods were developed for the quantification of 32 regulated and unregulated DBPs. A purge and trap (P&T) coupled with gas chromatography mass spectrometry (GC-MS) method was optimized that automated sample pre-treatment and analyzed volatile and semi-volatile compounds, including trihalomethanes (THMs), iodinated trihalomethanes (I-THMs), haloacetonitriles (HANs), haloketones (HKTs) and halonitromethanes (HNMs). LOQs were between 0.02-0.4 µg/L for most DBPs except for 8 analytes that were in the low µg/L range. A second method with liquid chromatography (LC) tandem mass spectrometry (MS/MS) was developed for the quantification of 10 haloacetic acids (HAAs) with a simple clean-up and direct injection. The LC-MS/MS direct injection method has the lowest detection limits reported (0.2-0.5 µg/L). Both methods have a simple sample pre-treatment, which make it possible for routine analysis. Hyperchlorination and uniform formation conditions (UFC) formation potential tests with chlorine were evaluated with water samples containing high and low TOC. Hyperchlorination formation potential test maximized THMs and HAAs while UFC maximized HANs. Ascorbic acid was found to be an appropriate quencher for both analytical methods. Disinfected drinking water from four water utilities in Alberta, Canada were also evaluated.     

Integration of solid phase extraction with HILIC-MS/MS for analysis of free amino acids in source water

Amino acids (AAs) are prevalent in source water, particularly during spring run-off. Monitoring of amino acids in source water is desirable for water treatment plants (WTP) to indicate changes in source water quality. The objective of this study was to establish analytical procedures for reliable monitoring of amino acids in source water. Therefore, we examined two different methods, large volume inject (LVI) and solid phase extraction (SPE), for sample preparation prior to HILIC-MS/MS. The LVI-HILIC-MS/MS method can provide fast and sensitive detection for clean samples, but suffers from matrix effects, resulting in irreproducible separation and shortening column lifetime. We have demonstrated that SPE was necessary prior to HILIC-MS/MS to achieve reproducible and reliable quantification of AAs in source water. A natural heterocyclic amine 1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid (MTCCA) was also included in the method to indicate changes in other natural nitrogenous compounds in source water. The SPE-HILIC-MS/MS method was able to achieve limits of detection from 2.6-3400 ng/L for the amino acids and MTCCA with RSDs (n=3) of 1.1%-4.8%. As well, retention times (RT) of the analytes were reproducible with variation less than 0.01 min (n=3) through the entire project. We further applied the SPE-HILIC-MS/MS method to determine AAs in authentic source water samples collected from two drinking water treatment plants (WTPs) during the 2021 spring run-off season. The results support that the SPE-HILIC-MS/MS method does not require derivatization and can provide reliable, accurate, and robust analysis of AAs and MTCCA in source water, supporting future monitoring of source water quality.     

校准曲线制备及应用中的一些问题

阐述了校准曲线的制备和应用，标准加入法，空白值参与回归，工作曲线和标准曲线的一些应注意的问题。