毛细管柱气相色谱法测定人血清中有机氯农药残留量

提出了毛细管气相色谱测定人血清中有机氯农药残留量的方法。利用正己烷超声提取人血清样品中有机氯农药六六六和滴滴涕,所得萃取液作气相色谱测定,用甲酸及浓硫酸净化、磺化处理后,电子捕获检测器检测。在优化的试验条件下,8种有机氯农药同分异构化合物组分在20 min内能够很好的分离,其质量浓度与色谱峰面积在0.4～10μg·L~(-1)浓度范围内呈线性关系,检出限(3S/N)在0.07～0.30μg·L~(-1)之间。方法的日内的相对标准偏差为2.9%～5.4%,日间的相对标准偏差为4.5%～8.9%。方法的加标回收率在81.5%～117.6%范围。     

气相色谱法同时测定土壤中10种有机氯农药残留量

运用气相色谱及内标法定量测定土壤中的七氯、艾氏剂、六六六及滴滴涕类等10种有机氯农药残留。测定结果的相对标准偏差为4．2％～22．0％,回收率为70．3%-119．0％。通过实样分析验证了方法的适用性。     

气相色谱法测定土壤中21种有机氯农药和4种有机磷农药

应用气相色谱法测定土壤中21种有机氯农药和4种有机磷农药(OCP′s及OPP′s)的含量。土壤样品(10g)以丙酮-正己烷(1+1)混合液(200mL)在65℃用索氏提取7h。提取液蒸缩至约2mL,用经固相萃取小柱净化。用上述混合液6mL分3次从柱上洗脱,洗脱液浓缩至1mL供气相色谱分析。测定OCP′s时用CLPⅡ型毛细管色谱柱分离,电子捕获检测器检测;测定OPP′s时用1701型毛细管色谱柱分离,火焰光度检测器检测。21种OCP′s和4种OPP′s在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.14~0.38μg·kg-1之间。加标回收率在68.0%~125%之间,测定值的相对标准偏差(n=10)在2.8%~5.9%之间。     

填充柱气相色谱法测定食品中有机氯农药

建立了测定食品中有机氯农药残留的气相色谱法。样品采用石油醚直接超声处理,在离心管中进行硫酸净化。α-666,γ-666、β-666、δ-666、p,p′-DDE、o,p′-DDT、p,p′-DDD、p,p′-DDT混合标准溶液各组分浓度为0.20~0.002μg/mL时,线性关系良好,相关系数大于0.999,RSD为2.92%~4.93%,回收率为86.1%~102.1%,检出限分别为0.0010、0.0015、0.0029、0.0021、0.0030、0.0078、0.0062、0.0066mg/kg。     

土壤中17种有机氯农药残留量的毛细管气相色谱测定法

采用专用索氏提取器、正己烷萃取、Elite-5MS弹性石英毛细柱分离、GC-ECD测定了土壤中17种有机氯农药残留量.方法的检出限为0.4×10-10～2.0×10-10 g,回收率范围在76.0%～108.9%之间,相对标准偏差为0.66%～9.10%.该方法适用于土壤有机氯农药残留量的分析.     

气相色谱法测定土壤中15种有机氯和多氯联苯

应用气相色谱法测定土壤中15种有机氯农药(OCP′s)及多氯联苯(PCB′s)。土壤样品(10g)用正己烷-丙酮(1+1)混合液160mL在65℃水浴中索氏提取4h,所得提取液用硫酸分次进行磺化净化。净化后的溶液氮吹浓缩至0.5mL,用正己烷定容至1mL。分取1μL进样,用HP-1色谱柱分离,用电子捕获检测器(ECD)检测。所测15种OCP′s和PCB′s的质量浓度均在1.0~100μg·L-1范围内与其峰面积呈线性关系,15种化合物的检出限(3S/N)在0.080~0.16ng·g-1之间。在空白样品中加入15种化合物的混合标准溶液10.0ng进行回收试验,测得回收率在86.4%~108%之间,其测定值的相对标准偏差(n=7)在2.4%~5.2%之间。     

气相色谱法测定橄榄油中22种有机氯农药

橄榄油样品用乙腈提取,提取液用氮气浓缩至近干,残留物用正己烷稀释,采用硫酸磺化净化。采用气相色谱法测定样品溶液中22种有机氯农药的含量,22种有机氯农药采用Inert Cap 17色谱柱(30m×0.25mm,0.25μm)分离,电子捕获检测器测定。22种有机氯农药的质量浓度在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.001～0.01mg·kg~(-1)。以空白样品为基体进行加标回收试验,所得回收率为70.8%～120%,测定值的相对标准偏差(n=6)为0.40%～16%。     

用微波消解气相色谱法测定鱼肉中的有机氯农药

研究了微波消解 -有机溶剂提取 -气相色谱法测定鱼肉样品中有机氯农药的分析方法。对消解液、微波辅助加热条件及提取溶剂进行了优化实验 ,选择冰醋酸 -高氯酸 (体积比4∶1)在600W微波功率下接受辐射2min分解鱼肉样品 ,用30 % (φ)苯的石油醚溶液提取 ,对各种有机氯农药的回收率除 p,p′_DDT为60.3 %外 ,其余均在83.4 %～109.6 %之间 ,与水浴加热分解的国家标准方法相当。该法具有快速 ,灵敏度、精确度、准确度高等优点 ,适用于大批量食品和生物样品中有机氯农药的分析测定。     

气相色谱法测定火锅底料中的多种有机氯农药和拟除虫菊酯农药残留

建立了火锅底料中21种有机氯农药和6种拟除虫菊酯农药残留的同时测定方法.样品经乙腈超声提取,凝胶渗透色谱、弗罗里硅土固相萃取柱和N-丙基-2-乙二胺净化,毛细管气相色谱柱分离后,微电子捕获检测器检测.火锅底料中有机氯农药和拟除虫菊酯农药的检出限分别为0.082～2.3 μg/kg和1.5～13.0 μg/kg;有机氯农药的加标水平为10, 20和50 μg/kg,拟除虫菊酯农药为20, 40和100 μg/kg时,27种农药的平均回收率为70.5%～116.0%;相对标准偏差为0.2%～6.1%.本方法快速、灵敏、可靠,可用于火锅底料中多种农药残留的同时检测.     

毛细管气相色谱法测定食品、中药中的有机氯农药

建立食品和中药中有机氯农药残留量的毛细管气相色谱检测方法。样品经有机溶剂超声提取,硫酸净化,采用OV-1701毛细管柱,不分流分流进样,程序升温分离,电子捕获检测器检测,外标法定量,平均回收率为84.3%~100.6%,RSD为1.28%~3.56%。该法操作简便,重复性及分离效果好。     

土壤中多种有机氯及拟除虫菊酯类农药的GC-ECD测定

气相色谱法同时测定土壤中多种有机氯及拟除虫菊酯类农药。对土壤的分析结果：有机氯农药的检出限0．001～0、003μg／mL，拟除虫菊酯类农药检出限0.008～0．02μg／mL，线性相关系数0．9978～0．9999。用y（石油醚）：V（丙酮）=3：1超声波提取，有机氯农药回收率94．2％～124．0％，相对标准偏差为3．3％～8．8％（n=5）；拟除虫菊酯类农药回收率95．2％～118．3％，相对标准偏差为5．7％～7．1％（n=5）；方法适用于土壤样品中农药残留测定。     

毛细管气相色谱法测定芝麻中多种有机磷农药残留量

建立了芝麻中多种有机磷农药残留量的毛细管气相色谱的测定方法。样品以V(乙腈 )∶V(丙酮 ) =1 0∶1混合溶剂为提取剂 ,应用超声波辅助提取 ,固相吸附层析柱净化m(中性氧化铝 )∶m(弗罗里硅土 ) =1∶1 ,采用GC FPD法同时测定芝麻中的多种有机磷农药残留量。检出限为 0 .0 1 1～ 0 .0 1 7μg mL。方法的回收率为 82 .1 %～ 1 0 9.7%。     

气相色谱-火焰光度法测定土壤中有机磷农药残留

建立了气相色谱-火焰光度(GC-FPD)分析土壤中敌敌畏、氧化乐果、二嗪农、乐果、甲基对硫磷、马拉硫磷、对硫磷、水胺硫磷、喹硫磷等9种有机磷农药残留量的方法。样品用丙酮-二氯甲烷(1:3)提取,浓缩、定容后用Hp-5MS(30m×0.25 mm×0.25μm)毛细管柱分离,FPD检测器检测。方法回收率在68.71%～110.39%之间;RSD在5.5%～11%之间;检出限在0.397～1.60μg/mL之间,方法可用于环境土壤样品中有机磷农药残留的测定。     

Fast solid phase extraction of polychlorobiphenyls and chlorinated pesticide residues from mussels using sep-pak cartridges

Summary A rapid method for the determination of chlorinated pesticides and polychlorinated biphenyls in mussels (Mytilus sp.) is reported. The mussel sample is homogenized and extracted with acetonitrile. The organic solution is concentrated and successively diluted with distilled water solution (12 g L⁻¹ NaCl). The organic compounds from water solution are adsorbed onto a NH₂ Sep-Pak cartridge. The clean-up step, in which the polychlorobiphenyls and chiorinated pesticides are separated in different eluates, is achieved by passing 25 mL of a 40% methanol aqueous solution through the NH₂ Sep-Pak and the C₁₈ Sep-Pak cartridges connected in series. The polychloroblphenyls are desorbed from the NH₂ Sep-Pak cartridge whilst the chlorinated peslicides are recovered from the C₁₈ Sep-Pak cartridge. In the separation of polychlorobiphenyls from the chlorinated pesticides tested in this work, only aldrin, hepatachlor and 4,4′-DDD are partially adsorbed with the polychlorobiphenyls onto the NH₂ Sep-Pak cartridge. The average recovery is ≥95.0% with a relative standard deviation ≤5.0%. The limits of detection for different pesticides and polychlorobiphenyl congeners are 0.01 and 0.008 μg Kg⁻¹. The final determination is carried out by capillary gas chromatography with ECD.     

Rapid determination of organochlorine pesticide residues in feeds by capillary gas chromatography

A simple micro-method is described for determination of 15 organochlorine pesticide residues in mixed feeds. Clean-up of the petroleum ether extract is by basic alumina minicolumn chromatography and quantitative identification is by capillary gas chromatography with electron capture detection. Cyanopropyl-polysiloxane chemically bonded fused silica capillary columns have been used to perform high resolution analyses in short time as well as to overcome possible interferences by PCBs. Recovery, repeatability, and detection limits of the proposed procedure are checked and results are also reported for non random samples of 180 feeds collected in Italy.     

固相萃取-气相色谱法检测茶叶中的有机磷农药残留量

建立了茶叶中22种有机磷农药的残留量的气相色谱分析方法. 样品用V(乙腈)∶V(丙酮)＝4∶1提取, 经Envi-Carb固相小柱净化, 以V(乙腈)∶V(甲苯)＝3∶1洗脱, GC-FPD检测, 外标法定量. 在添加0.05～1.0 mg/kg的水平, 22种有机磷的平均回收率在81.3%～107.9%之间, 相对标准偏差在1.1%～8.9%, 该方法的检出限为0.01～0.04 mg/kg. 该方法的灵敏度、准确度和精密度均符合农药残留量测定的技术要求.     

Headspace analysis of chlorinated organic solvents in aerosol cans by gas chromatography

Summary A gas chromatographic (GC) method for the analysis of chlorinated solvents in chemical products in aerosol cans is described. Conditions for the sampling of chemical products from aerosol cans were optimized, so that the recovery of the solvents was better than 90%. Chlorinated solvents were identified by headspace GC—electron capture detection (ECD) as well as by GC — mass spectrometry. Headspace analysis employing the standard additions method and GC-ECD was used for the quantitation of chlorinated solvents. Analysis of 159 acrosol products, for various uses, revealed that 9% of these did not comply with the Danish Aerosol Regulations. The results of the study further indicated that aerosol products for haircare, paints and paint removers, and many others, can be formulated without chlorinated solvents.     

超声波提取-固相萃取净化-气相色谱法分析烟草中拟除虫菊酯类农药及氟节胺残留

建立了超声波提取-固相萃取净化-气相色谱联用测定烟草中多种拟除虫菊酯类农药及氟节胺残留量的方法。与现行标准方法相比,本方法前处理简单、快速、有机溶剂消耗量少,且增加了分析目标物的数量。8种拟除虫菊酯类农药及氟节胺在0.1、0.5和1μg/g三个加标水平的回收率为86%～111%,相对标准偏差为0.2%～4.1%,满足当前烟草农药残留的检测要求。     

气相色谱法测定地表水中拟除虫菊酯类农药残留

建立了气相色谱检测地表水样中痕量氯氟氰菊酯、氯氰菊酯、氰戊菊酯和溴氰菊酯农药残留的分析方法。水样经环己烷液液萃取、无水硫酸钠过滤,再用N-丙基乙二胺和无水硫酸镁净化,用氮气吹干浓缩,再用正己烷溶解,离心分离后取上清液进样,以气相色谱法测定4种拟除虫菊酯的含量。4种拟除虫菊酯化合物的质量浓度在5~200μg/L范围内与色谱峰面积成良好的线性关系,相关系数均大于0.999,方法检出限为0.03~0.09μg/L,模拟水样的平均加标回收率为98.0%~104.5%,相对标准偏差为0.89%~6.44%(n=6)。该方法操作方便、快速,结果准确、可靠,有机溶剂用量少,适用于水中拟除虫菊酯类农药残留的测定。     

Diol sep-pak cartridges for enrichment of polychlorobiphenyls and chlorinated pesticides from water samples; determination by GC-ECD

Summary Gas chromatography of polychlorinated biphenyls and chlorinated pesticides in water samples has been performed after adsorption from a 20–200-mL sample on to a cartridge containing 100 mg diol-bonded porous silica. The PCBs are desorbed with 500 μL ethyl acetate, which is concentrated and analysed by gas chromatography with electron-capture detection (GC-ECD). The average recovery of 0.1 ng mL⁻¹ PCB congeners from distilled water and from Aniene river water is≥95% (standard deviation≤2.8). Average recoveries of 25 ng mL⁻¹ Aroclor 1254 from distilled water and from Aniene river water were, respectively, 94.4% and 92.5% (standard deviation 5.8). In the separation of PCB congeners from the chlorinated pesticides only the aldrin (40%) was eluted with the PCBs from the diol Sep-Pak cartridge by aqueous methanol. The method described is simple and reproducible.