A method was developed for determination of 7 indictors the polychlorinated biphenyls (PCBs) residues in porphyra by gas chromatography (GC) with electron capture detector (ECD). The PCBs were extracted with hexane/me...A method was developed for determination of 7 indictors the polychlorinated biphenyls (PCBs) residues in porphyra by gas chromatography (GC) with electron capture detector (ECD). The PCBs were extracted with hexane/methylene chloride (1:1, v/v) by ultrasonic extraction and the samples were cleaned up by concentrated sulfuric acid and Alumina-N solid phase extraction cartridge. The analytes were quantified by an internal standard method. Under optimal experimental conditions, good linearity was observed in the range of 5 - 200 ng/mL and the correlation coefficients were 0.9994 - 0.9998. The limit of quantitation (LOQ) for target analytes ranged from 6.0 to 10.0 μg/kg. At the spiked levels of 10, 50, 100 μg/kg, the average recoveries ranged from 90.9% to 102% with the relative standard deviations 2.12% - 6.32%. The result showed that the proposed method was rapid, and could be used for the determination of the PCBs in porphyra.展开更多
The extracted fish samples (w/w) using pressurized liquid extraction (PLE) were cleaned up by applying different adsorbent materials such as: combination of acidic/ basic silica and alumina, florisil, and silica gel e...The extracted fish samples (w/w) using pressurized liquid extraction (PLE) were cleaned up by applying different adsorbent materials such as: combination of acidic/ basic silica and alumina, florisil, and silica gel either alone or in combination with another sort of sorbent. Different solvents such as hexane (H), dichloromethane (DCM), with different compositions were used to elute the PCBs target compounds from the spiked fish samples. Overall the mean percentage recoveries for all PCBs congeners using PLE were ranging from 78.6% to 98.7%;from 79.4% to 91.8%;from 65.8% to 104.5% and from 82.4% to 100.9% for cases A, B, C, D and E, respectively. However, the overall mean percentage recoveries for the 13C-PCBs surrogate including: 101, 138, 153, 180 and 209 were ranging from 88.2% to 97.6%;from 79.4% to 90.2%, from 88.3% to 96.4%, from 79.8% to 90.4% and from 83.9% to 95.9%, for cases A, B, C, D and E, respectively. The limits of detection of the proposed method were varied from 0.01 to 0.28 ng/g (w/w) for different PCBs congeners. The proposed method has linear dynamic range from 21.5 ng/g to 109 ng/g. This method was applied to fish samples for the determination of the target PCBs components.展开更多
A modified separation method has been developed for determinating polychlorinated biphenyl congeners in environmental samples. Direct treatment of extract with concentrated HzSO4 was employed in the first step for rem...A modified separation method has been developed for determinating polychlorinated biphenyl congeners in environmental samples. Direct treatment of extract with concentrated HzSO4 was employed in the first step for removal of lipids and other interfering substances, then a joint column of alumina-silica gel(Ag+) was applied to separate PCBs fraction from HCH, DDT and its analogs. After this separation, the PCBs fraction was analyzed by capillary gas chromatography with ECD detector and confirmed by GC/MS. The recoveries of individual congeners in Aroclor 1254 through the separation are about 79%-84%. The method is very efficient and useful for determination of trace amount of PCB congeners in environmental samples.展开更多
建立了快速测定牛奶中20种多氯联苯（PCBs）和多环芳烃（PAHs）的气相色谱-串联质谱（GC-MS/MS）分析方法。目标化合物用正己烷提取3次,Cleanert Ba P-SPE固相萃取柱净化,GC-MS/MS测定。结果表明,20种目标物在5~200μg/L范围内呈良好线...建立了快速测定牛奶中20种多氯联苯（PCBs）和多环芳烃（PAHs）的气相色谱-串联质谱（GC-MS/MS）分析方法。目标化合物用正己烷提取3次,Cleanert Ba P-SPE固相萃取柱净化,GC-MS/MS测定。结果表明,20种目标物在5~200μg/L范围内呈良好线性,线性相关系数均大于0.99,方法定量下限为1.0μg/kg。在1.0,2.0,5.0μg/kg 3个加标水平下的平均回收率为67.3%~106.9%,相对标准偏差（RSD）为3.1%~13.9%。该方法简便、快速、准确,可用于牛奶中多氯联苯和多环芳烃残留的检测,为牛奶的质量控制和安全评价提供了保证。展开更多
文摘A method was developed for determination of 7 indictors the polychlorinated biphenyls (PCBs) residues in porphyra by gas chromatography (GC) with electron capture detector (ECD). The PCBs were extracted with hexane/methylene chloride (1:1, v/v) by ultrasonic extraction and the samples were cleaned up by concentrated sulfuric acid and Alumina-N solid phase extraction cartridge. The analytes were quantified by an internal standard method. Under optimal experimental conditions, good linearity was observed in the range of 5 - 200 ng/mL and the correlation coefficients were 0.9994 - 0.9998. The limit of quantitation (LOQ) for target analytes ranged from 6.0 to 10.0 μg/kg. At the spiked levels of 10, 50, 100 μg/kg, the average recoveries ranged from 90.9% to 102% with the relative standard deviations 2.12% - 6.32%. The result showed that the proposed method was rapid, and could be used for the determination of the PCBs in porphyra.
文摘The extracted fish samples (w/w) using pressurized liquid extraction (PLE) were cleaned up by applying different adsorbent materials such as: combination of acidic/ basic silica and alumina, florisil, and silica gel either alone or in combination with another sort of sorbent. Different solvents such as hexane (H), dichloromethane (DCM), with different compositions were used to elute the PCBs target compounds from the spiked fish samples. Overall the mean percentage recoveries for all PCBs congeners using PLE were ranging from 78.6% to 98.7%;from 79.4% to 91.8%;from 65.8% to 104.5% and from 82.4% to 100.9% for cases A, B, C, D and E, respectively. However, the overall mean percentage recoveries for the 13C-PCBs surrogate including: 101, 138, 153, 180 and 209 were ranging from 88.2% to 97.6%;from 79.4% to 90.2%, from 88.3% to 96.4%, from 79.8% to 90.4% and from 83.9% to 95.9%, for cases A, B, C, D and E, respectively. The limits of detection of the proposed method were varied from 0.01 to 0.28 ng/g (w/w) for different PCBs congeners. The proposed method has linear dynamic range from 21.5 ng/g to 109 ng/g. This method was applied to fish samples for the determination of the target PCBs components.
文摘A modified separation method has been developed for determinating polychlorinated biphenyl congeners in environmental samples. Direct treatment of extract with concentrated HzSO4 was employed in the first step for removal of lipids and other interfering substances, then a joint column of alumina-silica gel(Ag+) was applied to separate PCBs fraction from HCH, DDT and its analogs. After this separation, the PCBs fraction was analyzed by capillary gas chromatography with ECD detector and confirmed by GC/MS. The recoveries of individual congeners in Aroclor 1254 through the separation are about 79%-84%. The method is very efficient and useful for determination of trace amount of PCB congeners in environmental samples.
文摘建立了快速测定牛奶中20种多氯联苯（PCBs）和多环芳烃（PAHs）的气相色谱-串联质谱（GC-MS/MS）分析方法。目标化合物用正己烷提取3次,Cleanert Ba P-SPE固相萃取柱净化,GC-MS/MS测定。结果表明,20种目标物在5~200μg/L范围内呈良好线性,线性相关系数均大于0.99,方法定量下限为1.0μg/kg。在1.0,2.0,5.0μg/kg 3个加标水平下的平均回收率为67.3%~106.9%,相对标准偏差（RSD）为3.1%~13.9%。该方法简便、快速、准确,可用于牛奶中多氯联苯和多环芳烃残留的检测,为牛奶的质量控制和安全评价提供了保证。
