超高效液相色谱三重四级杆质谱联用法测定水中的氯霉素

建立了固相萃取一超高效液相色谱三重四级杆质谱联用法同时测定水中痕量的氯霉素残留,该方法采用电喷雾电离源、多重反应监测负离子模式在5min内完成对氯霉素的分析,方法检出限为0．2ng/L,空白样品和实际样品的加标回收率为76．2％～104％,该方法具有操作简便,灵敏度高,重现性好的特点。     

深圳市宝安区环境空气有机污染现状研究

采用热脱附和气相色谱-质谱联用技术研究了深圳市宝安区环境空气中挥发性有机物的组成,从中鉴定出18种有机化合物,并通过对其中5种苯系物的定量分析结果,讨论了宝安区环境空气有机污染状况。     

气袋采样-苏玛罐转移-GC/MS法测定废气中醛类恶臭物质

采用气袋采样-苏玛罐转移-GC/MS法测定废气中5种醛类恶臭物质,醛类同分异构体能够被完全分离、定性定量。保存时间验证试验表明,5种低浓度醛类在Tedler采样袋和PVDFs采样袋中能稳定存放12 h,高浓度醛类能较稳定地保存24 h,转移至苏玛罐中的样品能够稳定存放至少14 d。方法在4×10~(-10)～2×10~(-8)范围内线性良好,方法检出限为0.127μg/m~3～0.207μg/m~3,混合标气6次测定结果的RSD为3.4%～8.8%,加标回收率为103%～114%。     

固相微萃取技术在苯胺等突发性水环境污染事故中的应用

建立了固相微萃取与车载气相色谱-质谱联用技术现场快速定量分析突发性水环境污染事故中的硝基苯、苯酚、苯胺3种半挥发性有机物的方法。选用PA萃取纤维,调节水样p H为8.5,加入30%的氯化钠,45℃顶空萃取30 min可得最佳萃取效果。在最佳实验条件下,硝基苯、苯酚、苯胺的方法检出限分别为0.68、3.2、4.88μg/L;平行测定7次的相对标准偏差分别为5.37%、8.31%、2.86%;3种化合物的相关性系数均大于0.99;对实际样品测定的加标回收率在61.1%~120%。     

大气VOCs快速测定及其在环境空气污染应急溯源中的初步应用

突发性大气环境污染事件处于高发期,针对环境应急监测时效性强的特点,用便携式GC-MS快速测定大气中23种VOCs,探讨大气中VOCs测定在环境空气污染应急溯源中的应用。该方法在20.0μg/m3~3 200μg/m3范围内线性良好,按采样1 L计算,方法检出限为2.6μg/m3~9.4μg/m3,加标回收率为91.3%~103%,测定结果的RSD≤10.5%。将该方法用于突发性环境污染应急事件大气中VOCs的快速测定,通过对照企业特征污染物名录,能快速锁定污染源头。     

气相色谱-质谱联用法测定水中卤代乙酸类化合物

采用气相色谱-质谱联用法测定水中9种卤代乙酸类化合物,通过优化试验条件,使方法在5.00μg/L~200μg/L范围内线性良好。当取样量为40 m L时,方法检出限在0.7μg/L~1.0μg/L之间,3种实际水样的加标回收率为81.2%~98.0%,6次平行测定结果的RSD≤12%。     

鱼类样品中有机磷阻燃剂分析方法的优化研究

建立了鱼类组织样品中有机磷阻燃剂（OPFRs）的分析方法,优化了萃取条件、净化条件、液相色谱条件和质谱检测参数。确定了生物样品经冷冻干燥后,以1∶1（V/V）的正己烷/二氯甲烷混合溶液进行加速溶剂萃取,利用氨基固相萃取柱进行净化,以1∶1（V/V）的正己烷/二氯甲烷、二氯甲烷和9∶1（V/V）的二氯甲烷/甲醇为洗脱液,最后用超高效液相色谱-串联质谱同时对9种OPFRs进行定性定量检测。结果表明,各物质的基质加标回收率均为56.5%~108%,方法的测定下限为0.016~0.104 ng/g （以脂重计）,满足了生物样品中OPFRs的分析检测要求。利用该方法测定了北京和广州市养殖和野生鲫鱼肌肉组织样品,主要的OPFRs同族体为磷酸三正丁酯（TNBP）、磷酸三乙基己基酯（TEHP）、磷酸三（1-氯-2-丙基）酯（TCIPP）和磷酸三氯乙基酯（TCEP）,质量比为5.94~33.7 ng/g（以脂重计）,显示出良好的适用性。     

固相微萃取-便携式GC/MS快速测定水中痕量有机磷农药

采用固相微萃取-便携式气相色谱/质谱联用法（In situ SPME/GC-MS）分析地表水和废水中6种有机磷农药,通过优化测定条件,使6种有机磷农药在200 μg/L~500 μg/L范围内线性良好。方法检出限为033 μg/L～122 μg/L,低、高质量浓度标准溶液6次测定结果的RSD为68%~175%,加标回收率为849%~109%,与实验室方法的测定结果基本一致。     

LC-MS/MS method validation for determination of selected neonicotinoids in groundwater for the purpose of a column experiment

The work was carried out to develop and validate a method based on liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous detection and quantification of five neonicotinoid insecticides: acetamiprid, clothianidin, imidacloprid, thiacloprid and thiamethoxam in groundwater samples for the purpose of a further column experiment. This experiment will be used to analyze breakthrough curves of neonicotinoids under a saturated water flow to set transport parameters, where the reliability of the results of chemical analysis plays an important role. The validation was performed in a concentration range from 0.09?µg L^?1 to 100?µg L^?1 using an Infinity 1290 (Agilent, USA) chromatograph coupled with a QTrap 5500 mass spectrometer (Sciex, Canada). The calibration curves were obtained on the basis of the results of six standard solution analyses. Linearity was not lower than 0.998. The limit of detection was set at the lowest concentration which can be determined with an acceptable accuracy and precision. All pesticides had recoveries in the range 85–109% with relative standard deviation values less than 8.1%. The estimated measurement uncertainty did not exceed 30%, so the LC-MS/MS method fits for the intended purpose.     

Organic contamination of Italian and Tunisian culinary herbs and spices

Contaminants belonging to various classes, as polychlorobiphenyls, polycyclic aromatic hydrocarbons, organochlorine pesticides, organophosphorous pesticides, pyrethroid insecticides, fungicides, herbicides, synergists, carbamates, acaricides and insect growth regulators were simultaneously analysed by GC-MS/MS in 118 Italian and Tunisian culinary herbs and spices. The results obtained in Italian samples shown that laurel samples were the most contaminated with the presence of 15 residues on 140, whereas in rosemary (max value of 35?ng/g for cis-chlorfenyvinphos) and oregano (max value of 118.16?ng/g for ethion) some occasional residues can be observed, but always lower than the maximum residue levels; all the others samples shown no contamination. Among Tunisian samples, only rosemary contains a notably high content of pollutants exceeded the EU maximum residue limits (i.e., alachlor and phosalone with level of 359.2 and 43.3?ng/g, respectively), while oregano was determined to be free of contaminant residues. Considering the comparison among the different organic pollutants in Italian and Tunisian spices and herbs evaluated and the differences observed in this study a harmonization of regulation on contaminant residues in herbs and spices for human consumption should be needed, considering their increased use in diet and cooking.