加速溶剂萃取-高效液相色谱法测定固体废物中多环芳烃

建立了固体废物中多环芳烃的快速溶剂萃取(ASE)-高效液相色谱(HPLC)检测方法。加速溶剂萃取仪在温度100℃、压强1.05 MPa条件下,以体积比1:1的丙酮和二氯甲烷为萃取剂,萃取5 min,萃取液采用固相萃取柱或凝胶色谱净化。灰渣和污泥中的PAHs的方法检出限分别为1.03~1.96 μg/kg和4.71~7.04 μg/kg,相对标准偏差分别为4.0%~13.8%和3.3%~13%,加标回收率分别为73.2%~89.8%和67.7%~90.5%。     

微波萃取-气质联用测定土壤中的16种多环芳烃

用丙酮-正己烷(1:1体积比)混合溶剂,通过微波萃取法提取土壤中的16种多环芳烃组分。萃取溶液经硅胶小柱净化,最后用气相色谱-质谱法分析。以石英砂为基体进行加标回收测定。16种多环芳烃的检测限为0.18～0.53μg/kg,经精密度试验,相对标准偏差均5%,回收率在75.5%～108%之间。     

串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的邻苯二甲酸酯与多环芳烃

建立了用微波萃取(MAE)、固相萃取(SPE)净化、气相色谱,串联四极杆质谱(GC-QqQ-MS/MS)多反应监测同时测定土壤中16种多环芳烃和18种邻苯二甲酸酯的方法.通过优化前处理与分析条件,样品加标浓度在5μg/kg时的平均回收率在66.59%～122.07%之间,相对标准偏差均小于20%,邻苯二甲酸酯的检出限在0.04.0.84.ttg/kg之间.定量限在0.13～2.81μg/kg之间;多环芳烃的检出限在0.01～0.54μg/ks之间,定量限在0.02～1.81μS/kg之间,能够满足大量样品快速准确分析的需要.     

气相色谱法测定柑橘和土壤中螺螨酯残留

以丙酮为提取剂,二氯甲烷为萃取剂,采用弗罗里硅土柱净化,气相色谱-电子捕获检测器测定柑橘和土壤中的螺螨酯残留,优化了样品前处理条件。方法在0.141μg/L～5.65 mg/L范围内线性良好,最低检出限为0.003 5 mg/kg,空白样品在0.050 mg/kg、0.500 mg/kg、1.00 mg/kg 3个添加水平上的平均回收率为82.2%～110%,平行测定的RSD为2.6%～9.8%。     

SPE-GCMS法分析饮用水源水中痕量半挥发性有机物

采用C 18固相萃取柱富集,乙酸乙酯、二氯甲烷和丙酮混合溶剂以1∶1∶1比例洗脱、自动固相萃取的前处理方法,气相色谱质谱连用,分析水源水中33种半挥发性有机物,并与液液萃取前处理方法进行比较。结果表明:在500~5 000μg/L范围内,33种SVOC线性良好,相关系数0.990,回收率为70.1%~114.2%,相对标准偏差为2.4%~13.4%,方法检出限为0.06~0.25μg/L;而且该方法较液液萃取,检出样品种类多。适用于饮用水源水中半挥发性有机物的监测。     

加速溶剂萃取-固相萃取净化-高效液相色谱法测定玉米作物中多环芳烃含量

建立了加速溶剂萃取-固相萃取净化-高效液相色谱测定玉米作物中15种多环芳烃的方法,优化了试验条件.方法线性关系良好,15种多环芳烃的检出限在0.003 8～0.079μg/kg之间,空白加标试验的相对标准偏差在3.9%～11.7%之间,基质加标回收率在69.3%～115.3%之间.实际样品的测定结果表明,该方法分离效果...     

ASE萃取-SPE净化- HPLC法测定土壤中多环芳烃

建立了加速溶剂萃取-固相萃取净化-高效液相色谱测定土壤中16种多环芳烃的方法,优化了试验条件.方法线性关系良好,16种多环芳烃的检出限在0.412 ng/g～3.974 ng/g之间,空白加标试验的相对标准偏差在1.2%～12.7%之间,基质加标回收率在60.4%～126%之间.实际样品的测定结果表明该方法分离效果好,能够满足土壤分析的要求.     

微波萃取-高效液相色谱法测定环境空气总悬浮颗粒物中16种多环芳烃

用丙酮/正己烷(1∶1)混合溶剂,微波萃取法提取环境空气总悬浮颗粒物(TSP)中16种多环芳烃组分,各组分萃取率为66%～83%,萃取效果较好。高效液相色谱法二极管阵列检测器和荧光检测器串联可同时测出16种多环芳烃组分。在二极管阵列检测器响应的组分检测限为2 5μg/L～5 0μg/L,荧光检测器响应的组分检测限为0 01μg/L～0 1μg/L。对25μg/L16种多环芳烃标液作精密度试验,相对标准差均<5%,精密度好。取两个交通干线环境空气样品作TSP中多环芳烃测定,16种组分中除蒽、茚并(1,2,3cd)芘、芘、苊烯4种组分外,其他12种组分均有检出。     

固相净化气相色谱法测定水产品中多种有机磷农药残留

建立了水产品中8种有机磷农药残留同时测定的方法，选择乙腈提取，ENVI-C18串联PSA固相萃取柱净化，经丙酮/正己烷混合溶液（体积比1∶1）洗脱，洗脱液氮吹浓缩后采用气相色谱外标法定量。8种有机磷农药在0.050 mg/L～1.00 mg/L范围内线性良好，检出限在1.8 μg/kg～2.5 μg/kg之间，3个添加水平加标样品平行测定的相对标准偏差为1.1%～5.7%，回收率为69.8%～116%。     

高效液相色谱法测定土壤中多环芳烃的条件优化

研究了加速溶剂萃取(ASE)、固相萃取柱净化(SPE)、高效液相色谱仪(HPLC)联合测定土壤中16种多环芳烃(PAHs)的分析方法,选择以正己烷/丙酮(1+1,V/V)作为ASE提取溶剂,提取液经SPE硅胶小柱净化,正己烷/二氯甲烷(1+1,V/V)进行洗脱,洗脱体积为10 m L,洗脱液经旋转蒸发浓缩至近干,过0.22μm有机滤膜,用乙腈定容至1 m L,最后用HPLC-紫外检测器对提取液中16种PAHs进行定量分析。土壤中16种PAHs的方法检出限为2.8~4.9μg/kg,加标回收率为81.9%~102%,相对标准偏差为2.5%~6.2%,完全满足土壤中PAHs分析的质量控制要求,该法稳定性好、准确度高、可操作性强,适合于土壤样品中16种PAHs的准确测定。     

多环芳烃测定中净化方法的研究

对多环芳烃测定中的净化方法进行研究，为了选出最佳净化柱，在一定条件下分别采用硅胶LC-Si、弗罗里LC-Florisil和C18固相萃取净化柱对一定浓度的多环芳烃标准溶液进行净化，测定吸附后流出液多环芳烃浓度，计算吸附率；测定洗脱后流出液多环芳烃浓度，计算洗脱率。测定结果为硅胶、弗罗里和C18固相萃取净化柱对多环芳烃的吸附率分别在87．1％～100％，99．5％～100％和96．6％～100％之间，洗脱率分别在0～106％，78．7％．109％和79．0％～115％之间。结果表明，GC／MS内标法测定样品中多环芳烃使用最理想的净化柱为弗罗里净化小柱，其次为C18净化小柱，最后为硅胶净化小柱。     

超声波萃取-气相色谱/质谱法测定土壤中15种Pops类有机氯农药

用探头式超声波萃取仪、己烷/丙酮混合溶剂提取土壤中的15种Pops类有机氯农药(包括六氯苯、七氯、六六六、氯丹、艾氏剂、狄氏剂、异狄氏剂、灭蚁灵、滴滴涕),萃取溶液经氟罗里硅土柱净化、氮吹浓缩,用气相色谱/质谱仪(GC-MS)进行测定。方法检出限0.4～1.4μg/kg,空白样品有机氯农药加标回收率为52.8%～118%、有机氯标记替代物回收率为71.0%～122%,RSD为6.8%～16.5%。     

超声波萃取- GC/MS法测定土壤中多氯联苯

建立了超声波萃取、氟罗里硅土柱净化、气相色谱/质谱联用选择离子扫描模式测定土壤样品中多氯联苯Arochlor系列的方法.方法线性良好,灵敏度高,RSD为9.5%～12.2%,加标回收率为65.0%～105%,标准土壤样品的测定结果也符合要求.     

土壤和河流沉积物中六六六和滴滴涕残留的测定

采用密闭微波提取、超声波提取、索氏提取对土壤和河流沉积物进行前处理,提取液经弗罗里硅土柱净化或浓硫酸净化.通过回收率实验和精密度实验对三种提取方法和两种净化方法进行比较,建立了微波提取土壤和河流沉积物中六六六和滴滴涕,浓硫酸净化,气相色谱一质谱测定的分析方法,方法回收率在84%～110%之间,精密度(RSD)在2.8%～9.9%之间.采用该方法对阜阳市废弃农药厂周围的土壤和河流沉积物中六六六和滴滴涕进行了监测.     

Comparison of pressurized fluid extraction, Soxhlet extraction and sonication for the determination of polycyclic aromatic hydrocarbons in urban air and diesel exhaust particulate matter

In order to characterize and compare the chemical composition of diesel particulate matter and ambient air samples collected on filters, different extraction procedures were tested and their extraction efficiencies and recoveries determined. This study is an evaluation of extraction methods using the standard 16 EPA PAHs with HPLC fluorescence analysis. Including LC analysis also GC and MS methods for the determination of PAHs can be used. Soxhlet extraction was compared with ultrasonic agitation and pressurized fluid extraction (PFE) using three solvents to extract PAHs from diesel exhaust and urban air particulates. The selected PAH compounds of soluble organic fractions were analyzed by HPLC with a multiple wavelength shift fluorescence detector. The EPA standard mixture of 16 PAH compounds was used as a standard to identify and quantify diesel exhaust-derived PAHs. The most effective extraction method of those tested was pressurized fluid extraction using dichloromethane as a solvent.     

微波萃取-气相色谱法测定土壤中有机氯残留

采用微波萃取-硅镁吸附剂净化-气相色谱法测定土壤中有机氯农药，优化了试验条件。方法线性良好，8种有机氯农药的检出限为0.09ng／g-0.62ng／g，样品测定的RSD为2.6％-13.2％，基质加标平均回收率为93.7％-112％，质控样的测定结果与参考值相吻合。     

Distribution behavior and carcinogenic level of some polycyclic aromatic hydrocarbons in roadside soil at major traffic intercepts within a developing city of India

A study of polycyclic aromatic hydrocarbons (PAHs) pollution in roadside soil was conducted at a developing city locations of Jalandhar (Punjab), India in winter season to ascertain the contamination levels and their distribution behavior in roadside soil. PAHs concentration level of ten locations was measured at 1, 2, and 3 m distances from roadside soil covering all the major traffic intercepts within a city. Samples were extracted in acetone and dichloromethane (1:1) using soxhlet extraction. The extracts were filtered on a silica gel micro column to remove impurities and eluate was subjected to GC-FID. The total average PAHs concentration (city average) was found to be 4.04 μg g(-1), whereas the concentration of 16 individual PAHs was found to vary between 0.008 and 28.4 μg g(-1). The average concentration of noncarcinogenic and carcinogenic PAHs in all the samples was 2.17 and 6.41 μg g(-1) (ratio 1:2.95). The concentration of five ringed PAHs was found to be 45% to 60%, whereas two ringed PAHs were found to be in the range from 0.28% to 0.56% in all most all locations. The average highest PAHs concentration for any individual location was found as 12.23 μg g(-1) at DAV Chowk at 1 m distance and minimum concentration was 0.98 μg g(-1) at Maqsuda Chowk at 1 m distance from roadside. DiB (ah) A was the individual PAHs found in highest concentration in all the intercepts ranging between 1.26 and 28 μg g(-1). At most of the city intercepts, total carcinogenic PAHs concentration was found to range from 60% to 80% in comparison to noncarcinogenic PAHs (20%-40%) at most of the intercepts. The pollution level our study was compared with other cities of India/worldwide.     

Direct coupling of supercritical fluid extraction-supercritical fluid chromatography for the determination of selected polycyclic aromatic hydrocarbons in aqueous environmental samples

A rapid and simple method is described for the quantitative determination of polycyclic aromatic hydrocarbons in aqueous environmental samples. A microscale on-line supercritical fluid extraction-supercritical fluid chromatography system using carbon dioxide is employed. The extract is analysed using capillary supercritical fluid chromatography with UV detection. Detection was carried out at 254 nm. An extraction efficiency of as high as 91% was obtained for the PAHs.     

加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱测定土壤和沉积物中8种多溴联苯醚

建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1～100 ng/mL(BDE-209为10～1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004～0.1 ng/g,方法回收率为75%～110%,方法精密度为2.4%～15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。     

底质农残测定中固相柱净化体系的选择

使用固相柱对底质中的7种农残进行净化。结果表明,在相同淋洗条件下,使用氟罗里硅土柱比硅胶柱净化效果好。比较了不同溶剂体系、不同溶剂配比下2种萃取柱的净化效果,选择乙醚-正己烷(体积比1∶2)或丙酮-正己烷(体积比1∶4)作为净化溶剂,较小的收集体积都可满足所有目标化合物的回收率要求;相比较而言,丙酮-正己烷(体积比1∶4)作为净化溶剂,洗脱液的杂质干扰更小,净化效果更好。使用氟罗里硅土柱和丙酮-正己烷(体积比1∶4)对样品净化,方法简单,快速,净化效果好,适合大批量底质样品的前处理净化过程。