UPLC-MS/MS测定地表水中总微囊藻毒素的快速前处理方法探究

为方便地表水中总微囊藻毒素(TMCs)的预警监测,探究提取MC-LR、MC-RR、MC-YR的不同快速前处理方法,建立同时测定3种TMCs的煮沸-过滤-UPLC-MS/MS法.该方法在0.006μg/L～50.0μg/L范围内线性良好,方法检出限为0.006μg/L～0.010μg/L,实际水样3个质量浓度水平的加标回...     

秸秆燃烧产生的颗粒物中有机示踪物的分析方法

针对秸秆燃烧产生的颗粒物建立了测定4种有机示踪物的GC-MS分析方法,着重讨论了柱前衍生反应的条件,通过条件实验确定了在样品中加入80-100μl BSTFA/TMCS作为衍生试剂,在70℃下反应2h的最佳反应条件.方法的检测限为0.042-0.260μg,精密度为2.7%-19.7%,加标回收率为60.3%-111%.应用本方法定量分析了小麦秸秆闷烧排放的细颗粒物中22种有机物的含量,其分布特征为糖类物质含量最高,其次为含-OCH3酚类和甾醇类物质,而烷醇类物质含量最低.     

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.     

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-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.     

固相萃取-超高效液相色谱-串联质谱法同时测定地表水中9种性激素

建立了地表水中9种性激素的固相萃取-超高效液相色谱-串联质谱检测方法。利用HLB固相萃取柱富集水体中痕量性激素,用甲醇洗脱并浓缩,再以1 mmol/L氟化铵-乙腈为流动相,经C_(18)柱分离,采用电喷雾离子源、质谱多反应监测模式,内标法定量,实现了地表水中9种性激素的同时检测。方法检出限为0. 1～1. 8 ng/L,在低、中、高3个加标水平下,性激素的平均回收率为69. 6%～115. 0%,相对标准偏差为3. 2%～17. 7%。该方法灵敏度高,定性准确,操作简单高效,适用于地表水中9种性激素的定性定量分析。     

高效液相色谱串联质谱法分析土壤中多溴联苯醚类化合物

建立了一种超高效液相色谱串联质谱法(UPLC-MS/MS)同时测定土壤中8种多溴联苯醚化合物(PBDEs)的方法,采用快速溶剂萃取(ASE)和凝胶净化色谱(GPC),经BEH反相C₁₈色谱柱分离,10 min内完成分离,使用含0.1%氨水的甲醇和水进行梯度洗脱,采用液相色谱-负离子-大气压化学电离(APCI)串联质谱,多反应监测模式(MRM),加入 ¹³C₁₂-BDE-139和¹³C₁₂-BDE-209内标作定量分析。结果表明:在优化的分析条件下,PBDEs的线性相关系数为0.998 8～0.999 5,方法检出限为0.22～0.59 μg/kg,在2个添加水平下,平均回收率为71%～126%,标准偏差为3%～18%,土壤实际质控样测定结果均在允许范围内。适合于土壤中PBDEs的快速分析,特别对于高溴代PBDEs,相比气相色谱质谱方法具有更快的分析速度和更好的稳定性。     

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%。