高效液相色谱法检测植物油中苯并[a]芘的含量

建立并验证高效液相色谱法检测植物油中苯并[a]芘的含量.将植物油样品溶于正己烷中混匀,用苯并[a]芘固相萃取柱净化,用正己烷洗脱苯并[a]芘,荧光检测器检测.苯并[a]芘在0.1～100μg/kg浓度范围内线性相关系数r2=0.9999,本方法平均回收率为96.95%～101.30%,相对标准偏差RsD为0.980%～...     

超声提取-高效液相色谱法测定空气中苯并[a]芘

通过研究空气样品中苯并[a]芘的分析方法,确定了HPLC-FLD法的最佳分析条件,当流动相比例为乙腈/水(80∶20),流速1.0 m L/min,荧光检测激发波长293 nm,检测波长430 nm,提取溶剂为15 m L乙腈萃取3次时,获得了满意的分析结果。上述条件下,方法检出限为3×10-5μg/Nm3,回收率为96.6%~111.2%,精密度好(7.8%~10.1%,n=7),可以满足对空气样品中苯并[a]芘的日常监测分析。     

超声提取-高效液相色谱法测定空气中苯并[a]芘

通过研究空气样品中苯并[a]芘的分析方法,确定了HPLC-FLD法的最佳分析条件,当流动相比例为乙腈/水(80∶20),流速1.0 m L/min,荧光检测激发波长293 nm,检测波长430 nm,提取溶剂为15 m L乙腈萃取3次时,获得了满意的分析结果。上述条件下,方法检出限为3×10-5μg/Nm3,回收率为96.6%¹11.2%,精密度好(7.8%111.2%,精密度好(7.8%¹0.1%,n=7),可以满足对空气样品中苯并[a]芘的日常监测分析。     

磁固相萃取-HPLC测定环境空气中的苯并[a]芘

本文建立了磁性固相萃取结合高效液相色谱法测定环境空气中苯并[a]芘的新方法。空气滤膜中的苯并[a]芘经乙腈超声提取,20mg Fe_3O_4-SiO_2-G涡旋萃取,用1mL乙腈洗脱后经HPLC测定。结果表明,苯并[a]芘在0.02～2.0μg·mL~(-1)的浓度范围内具有良好的线性关系,相关系数R~2=0.9991,检出限为0.06ng·m~(-3),定量限为0.2ng·m~(-3),回收率为91.0%～102.2%,相对标准偏差为3.1%～8.2%,实际样品的分析结果与HJ956-2018的偏差≤10%。该法快速简便、灵敏度高、成本较低,具有良好的重现性和准确性,适用于大批量样品的检测分析,可做为环境空气中苯并[a]芘的日常监测方法,并为其它污染物的检测提供参考。     

高效液相色谱-荧光法快速测定茶籽油中苯并(a)芘的残留

建立了一种高效液相色谱-荧光法检测茶籽油中苯并(a)芘的分析方法。以市售的茶籽油作为供试样品,试样中的含有苯并(a)芘的样品加入氢氧化钾-无水乙醇溶液,在水浴加热皂化后用正己烷萃取,氮气吹干后以液相色谱-荧光检测器测定,外标法定量。乙腈和水(88∶12,V/V)为流动相,流速为1.0 m L/min,荧光检测器激发波长为384 nm,发射波长为406 nm,外标法峰面积定量。结果表明:苯并(a)芘在0.5~50.0 ng/m L范围内呈现良好的线性关系,相关系数0.9996,在3.0~60.0μg/kg添加水平时,加标回收率为79.53%~99.93%,相对标准偏差为0.11%~1.11%(n=6);方法的检出限和定量限分别为0.0686μg/kg和0.2284μg/kg。该方法测定茶籽油中的苯并(a)芘方便,快捷,准确可靠,易推广使用。     

气相色谱串联质谱法测定卷烟主流烟气中的B[a]P

建立了超声萃取-气相色谱-串联质谱法(GC-MS/MS)同时测定卷烟主流烟气中苯并[a]芘的分析方法。捕集了卷烟主流烟气总粒相物的剑桥滤片经环己烷超声萃取,在选择反应监测(MRM)模式下进行GC-MS/MS分析,内标法定量。结果表明:苯并[a]芘线性良好,r2为0.9996,方法的检出限(LOD)和定量限(LOQ)分别为0.4 ng/支和0.8 ng/支,加标回收率为98.2%~99.3%,相对标准偏差为1.7%~6.6%。该方法操作简便、灵敏,适合用于卷烟主流烟气"中苯并[a]芘释放量的测定。     

GC-MS法测定电子烟烟气中的苯并[a]芘

采用气相色谱-质谱联用法(GC-MS)测定电子烟烟气中的苯并[a]芘,电子烟样品在ISO标准抽吸模式,采用单层剑桥滤片对电子烟烟气释放物中的粒相部分进行捕集。待抽吸完毕后,将剑桥滤片以环己烷溶液超声萃取并浓缩用以测定。该方法中苯并[a]芘的检出限为4.5 ng/m L,定量限为15 ng/m L,样品中苯并[a]芘加标回收率在95.5%~97.6%之间。结果表明:该方法具有基质干扰少、定量准确、灵敏度高等特点。     

超高效液相-荧光检测器法测定柴油中多环芳烃

建立了采用超高效色谱(UPLC)-荧光检测器法测定柴油中10种常见的多环芳烃含量的方法。这10种常见的多环芳烃为萘、苊、二氢苊、芴、菲、蒽、荧蒽、芘、苯并[a]蒽、艹屈、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘和苯并[g,h,i]芘。样品经过固相萃取后用甲醇溶解,采用Acquity UPLC BEH Phenyl C18柱(100 mm×2.1 mm,1.7μm)分离,乙腈-水为流动相进行梯度洗脱,采用荧光检测器检测,并用外标法进行定量分析。结果表明,在一定质量浓度范围内,峰面积与质量浓度的线性关系良好,用标准加入法进行回收率实验,对方法的准确度进行考察,相对标准偏差为0.56%⁸.76%,加标回收率为100.04%8.76%,加标回收率为100.04%¹15.04%。与其他检测柴油中多环芳烃方法比较,该方法简单,分离效果好,快速及准确。     

高效液相色谱-荧光检测法测定贝类中15种多环芳烃

建立了高效液相色谱-程序荧光检测法同时测定贝类中15种多环芳烃的方法。通过液相色谱柱、荧光激发和发射波长等条件的优化,实现15种多环芳烃组分基线完全分离和荧光高灵敏度检测。在优化的实验条件下,检测的15种多环芳烃中萘、苊和芴的检出限为0.5μg/kg,苯并[b]荧蒽、二苯并[a,h]蒽和苯并[g,h,i]苝的检出限为2.0μg/kg,其余化合物的检出限为1.0μg/kg;在检测的15种多环芳烃中,菲、蒽、芘、苯并[a]蒽、崫、苯并[a]芘、茚并[1,2,3-cd]芘在0.001~0.5 mg/L浓度范围,其余化合物在0.002~1.0 mg/L浓度范围,呈良好的线性相关,相关系数r0.995;当样品加标水平分别为2、10、100μg/kg时,回收率在71.1%~98.4%,RSD10%。该检测方法重现性高,检测灵敏度和准确度均满足分析要求。     

超高效液相-荧光检测器法测定柴油中多环芳烃

建立了采用超高效色谱(UPLC)-荧光检测器法测定柴油中10种常见的多环芳烃含量的方法。这10种常见的多环芳烃为萘、苊、二氢苊、芴、菲、蒽、荧蒽、芘、苯并[a]蒽、艹屈、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘和苯并[g,h,i]芘。样品经过固相萃取后用甲醇溶解,采用Acquity UPLC BEH Phenyl C18柱(100 mm×2.1 mm,1.7μm)分离,乙腈-水为流动相进行梯度洗脱,采用荧光检测器检测,并用外标法进行定量分析。结果表明,在一定质量浓度范围内,峰面积与质量浓度的线性关系良好,用标准加入法进行回收率实验,对方法的准确度进行考察,相对标准偏差为0.56%~8.76%,加标回收率为100.04%~115.04%。与其他检测柴油中多环芳烃方法比较,该方法简单,分离效果好,快速及准确。     

Extraction of Polycyclic Aromatic Hydrocarbons in Barn Owls ( Tyto Alba ) from Northwest Spain by SFE and HPLC-FL Analysis

Supercritical fluid extraction (SFE) and high-performance liquid chromatography-fluorescence detection (HPLC-FL) were used to determine concentration of anthracene, benzo[ a ]anthracene, benzo[ a ]pyrene, benzo[ b ]fluoranthene, benzo[ ghi ]perylene, benzo[ k ]fluoranthene, chrysene, fluoranthene, pyrene, and indeno[1,2,3- cd ]pyrene in six classes of tissue (heart, liver, intestine, muscle, lung, and kidney) of 11 barn owls from Galicia (northwest Spain). We have detected fluoranthene and pyrene in >40.0% of samples, anthracene in 35.4%, and benzo[ a ]anthracene in 12.3%. Mean concentrations were between 0.398 w g/kg dry weight for anthracene and 4.855 w g/kg dry weight for fluoranthene. Lung and intestine tissues were more polluted than the other tissues.     

用聚合物试剂减少煤沥青中3,4-苯并芘的研究

研究了用聚合物同煤沥青反应降低其中3,4-苯并芘的方法。实验采用3种聚合物同煤沥青反应,得出不同的聚合物对减少3,4-苯并芘的作用效果,通过对聚苯乙烯-丁二烯-苯乙烯、古马隆-茚树脂和聚乙二醇的研究发现:添加4%的古马隆-茚树脂对煤沥青中3,4-苯并芘的脱除效果较好,脱除率达到46.78%,最佳反应温度为270℃,煤沥青中的3,4-苯并芘的质量分数由1.43%降低到0.76%。     

Major gaseous and PAH emissions from a fluidized-bed combustor firing rice husk with high combustion efficiency

This experimental work investigated major gaseous (CO and NO_x) and PAH emissions from a 400 kW_th fluidized-bed combustor with a cone-shaped bed (referred to as ‘conical FBC’) firing rice husk with high, over 99%, combustion efficiency. Experimental tests were carried out at the fuel feed rate of 80 kg/h for different values of excess air (EA). As revealed by the experimental results, EA had substantial effects on the axial CO and NO_x concentration profiles and corresponding emissions from the combustor. The concentration (mg/kg-ash) and specific emission (μg/kW h) of twelve polycyclic aromatic hydrocarbons (PAHs), acenaphthylene, fluorene, phenanthrene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene and indeno[1,2,3-cd]pyrene, were quantified in this work for different size fractions of ash emitted from the conical FBC firing rice husk at EA = 20.9%. The total PAHs emission was found to be predominant for the coarsest ash particles, due to the effects of a highly developed internal surface in a particle volume. The highest emission was shown by acenaphthylene, 4.1 μg/kW h, when the total yield of PAHs via fly ash was about 10 μg/kW h.     

溶剂效应对脱除煤沥青中3,4-苯并芘的影响

研究了单种溶剂、混合溶剂对3,4-苯并芘的溶解选择性及煤沥青溶解量。并以顺丁烯二酸酐为改性剂、硫酸为催化剂,考察了溶剂效应对降低煤沥青中3,4-苯并芘的影响。研究表明,环己烷、甲苯,环己烷、乙酸丁酯组成的混合溶剂具有较好的3,4-苯并芘溶解选择性和合适的煤沥青溶解量。当环己烷∶甲苯=2∶1（体积比）和环己烷∶乙酸丁酯=2∶1（体积比）为反应溶剂时,能够高效地脱除煤沥青中3,4-苯并芘,煤沥青中3,4-苯并芘降低率分别达到88.26%和90.83%。其原因认为是此类溶剂能使包裹在沥青颗粒内部的3,4-苯并芘释放出来,且3,4-苯并芘与改性剂能够形成均相反应体系,大部分不具有致癌性的高相对分子质量环芳烃与改性剂之间形成两相体系,从而提高了改性剂与3,4-苯并芘的有效反应。     

Contamination of Soil by Polycyclic Aromatic Hydrocarbons in Some Urban Areas

The contamination by 16 polycyclic aromatic hydrocarbons (PAHs) in surface soils, sampled at a 0-5 cm depth in the urban areas of Tallinn, Helsinki, Vilnius, Chicago, London is reported. All samples were analyzed using the same protocol. The median concentrations ( w g/kg) were found to be 117, 539, 127, 3,263, 1,728 for pyrene; 62, 236, 43, 1,634, 1,652 for benzo[ a ]pyrene; 86, 304, 92, 2,295, 2,068 for benzo[ a ]pyrene toxic equivalents, calculated using the benzo[ a ]pyrene toxic equivalency factors; 467, 1,471, 392, 8,981, 6,837 for a total of seven probable human carcinogenic PAHs: benzo[ a ]anthracene, chrysene, benzo[ b ]fluoranthene, benzo[ k ]fluoranthene, benzo[ a ]pyrene, dibenz[ ah ]anthracene, indeno[1,2,3- cd ]pyrene; 911, 2,941, 672, 16,183, 13,718 for the total of 16 PAHs, recommended by the U.S. Environmental Protection Agency: naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[ a ]anthracene, chrysene, benzo[ b ]fluoranthene, benzo[ k ]fluoranthene, benzo[ a ]pyrene, dibenz[ ah ]anthracene, benzo[ ghi ]perylene, indeno[1,2,3- cd ]pyrene in Tallinn ( n = 3), Helsinki ( n = 3), Vilnius ( n = 15), Chicago ( n = 4), London ( n = 3), respectively. The size of the population is a statistically significant factor in urban soil contamination by high-molecular-mass PAHs.     

Degradation of polycyclic aromatic hydrocarbons by hydrogen peroxide catalyzed by heterogeneous polymeric metal chelates

Chelating sorbents with 8-hydroxyquinoline (IVa), 8-hydroxyquinoline-5-sulfonic acid (IVb), and tris(2-aminoethyl)amine (VI) ligands immobilized on macroporous methacrylate matrix were prepared and saturated with Co(II), Cu(II), and Fe(II). All these chelates catalyze cleavage of H₂O₂ yielding highly reactive hydroxyl radicals. All were able to degrade by this mechanism polycyclic aromatic hydrocarbons (anthracene, benzo[a]pyrene and benzo[k]fluoranthene). The most effective catalysts IVa-Fe, IVb-Fe, and VI-Cu (25 mg with 100 μmol H₂O₂) performed complete decomposition of 33 μg anthracene and benzo[a]pyrene during one 7-day catalytic cycle at 25 °C. The fastest decomposition proceeded during the 1st day of incubation; 75% of anthracene and 74% of benzo[a]pyrene were decomposed by IVb-Co within the first 24 h. More than 25% decomposition within the 1st day was also achieved with IVb-Fe, VI-Cu, IVa-Cu, and VI-Co for anthracene and more than 30% benzo[a]pyrene was decomposed by IVb-Fe, VI-Cu, IVa-Cu, and IVb-Cu during the same period. 1,4-Anthracenedione was the main product of anthracene oxidation by all catalysts. The catalysts were stable at pH 2–11 depending on their structure and able to perform sequential catalytic cycles without regeneration.     

SAMPLING AND ANALYSIS OF POLYCYCLIC AROMATIC HYDROCARBONS IN URBAN AND RURAL ATMOSPHERES: SPATIAL AND GEOGRAPHICAL VARIATIONS OF CONCENTRATIONS

Atmospheric sampling (gas and particles) of PAHs (naphthalene, acenaphthene, fluorene, anthracene, phenanthrene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[j]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, benzo[ghi]perylene, dibenz[a,h]anthracene, indeno[1,2,3-cd]pyrene, coronene) on XAD-2 resin (20 g) and glass fiber filters respectively, were performed in 2002 by using Digitel DA80 high-volume samplers equipped with a PM10 head. Samplings were performed in Strasbourg (east of France) and its vicinity (Schiltigheim and Erstein). Sites were chosen to be representative of urban (Strasbourg), suburban (Schiltigheim), and rural (Erstein) conditions. Field campaigns were undertaken simultaneously in urban, and suburban, urban and rural sites during spring and autumn during 4 h at a flow rate of 60 m³/h^?1 which gives a total of 240 m³ · h^?1 of air per sample. The period of sampling varied between 06:00 to 10:00, 11:00 to 15:00, 17:00 to 21:00 in order to evaluate a variation of concentration during automobile traffic between urban, suburban, and rural areas. Gas and particle samples were separately Soxhlet extracted for 12 h with a mixture of CH₂Cl₂/n-hexane (50:50 v/v), concentrated to about 1 mL with a rotary evaporator and finally dried under nitrogen. Dry extracts were dissolved in 1 mL of CH₃CN before analysis. Before use, traps were Soxhlet cleaned for 24 h with the same mixture as used for the extraction. Analysis of each extract was performed by reverse phase HPLC, and fluorescence detection and quantification was done with respect to triphenylene used as internal standard. Results shows that automobile traffic seems to be the main source of PAHs in urban areas whatever the period (autumn and spring) while in autumn other sources, especially coming from combustion, influence the atmospheric contamination by PAHs.     

Degradation of Benzo[a]Pyrene as Sole Carbon Source by a Non White Rot Fungus,Fusarium Solani

Non white rot fungi isolated from fuel-contaminated soil were screened for their ability to grow with benzo[a]pyrene as sole carbon source. The capacity of one isolate identified as F. solani F33 was further investigated by studying the mineralization of [7,10-¹⁴C]benzo[a]pyrene. Spores of F. solani were able to germinate in presence of benzo[a]pyrene and growing mycelium mineralized [7,10-¹⁴C]benzo[a]pyrene (0.2% over a period of 10 days). The amount of ¹⁴CO₂ released decreased of 66% in 10 days culture in the presence of the inhibitor of cytochrome P-450 1-aminobenzotriazole, suggesting that such enzymes are involved in benzo[a]pyrene degradation by F. solani. This hypothesis was also enhanced by observing, in F. solani grown on benzo[a]pyrene, the presence of small vesicles with high