毛细管气相色谱法快速测定14种农药的有效成分

建立了用毛细管气相色谱法快速测定毒死蜱、三唑酮等14种农药的有效成分的分析方法,采用Rtx-1701(30 m×0.32 min×0.25 μm)和氢火焰离子化检测器(FID),内标法定量,气相色谱.质谱定性确证,样品的添加回收率为90.8%～104.6%,相对标准偏差为:0.09%～3.56%,该方法可作为测定单剂、复配制剂及多种农药制剂同时测定其有效成分的方法;方法能通过一次进样,同时鉴别出在分析的农药制剂中是否含有甲胺磷、久效磷、对硫磷、甲基对硫磷等禁止销售、使用的农药.     

毛细管柱气相色谱法测定土壤中的有机氯农药

研究了使用毛细管柱气相色谱法测定土壤中有机氯农药的分离条件、萃取方法、净化方法以及用替代品进行全程质量控制的方法。有机氯农药检出限在 1 .1～ 4.0 μg L之间 ,各化合物保留时间的RSD <0 .1 % ,所测定化合物的质量浓度在 0 .0 0 6～ 0 .2 0mg L范围内 ,各物质校正曲线 (浓度与峰面积 )的相关系数在 0 .992 6～ 0 .9971之间。用正己烷 丙酮 ( 1 1 ) 1 0 0mL超声波萃取 ,有机氯农药的萃取回收率在 96.3%～ 1 1 4% ,RSD为 0～ 1 1 %。用国产硅镁吸附剂净化 ,有机氯农药的回收率在 1 0 0 %～ 1 40 %之间 ,弗罗里硅土的回收率在 1 0 4 %～ 1 33%之间 ,硅镁吸附剂可以替代弗罗里硅土用于样品的净化。     

气相色谱法测定蔬菜中有机磷农药的残留量

采用DB-1型毛细管柱及氮磷检测器，建立了同时测定蔬菜中有机磷农药甲胺磷、氧化乐果、甲拌磷、甲基对硫磷残留量的气相色谱法，测定4种有机磷农药残留量的线性范围均为0．02-4．00mg／L，相关系数为0．9955～0.9980，检出限为0.0012～0．0020mg／L，加标回收率为89．3％-92．2％，相对标准偏差为2．2％～3．2％。     

大口径毛细管气相色谱法测定油脂、果蔬中20种有机氯农药的残留量

 对水果、蔬菜样品采用混合溶剂提取 ,对油脂样品则采用乙腈分配处理 ,然后运用柱色谱净化方式 ,以HP 1 0 1大口径弹性石英毛细管柱为分离柱 ,以电子捕获检测器检测 ,用气相色谱法测定油脂、水果、蔬菜中 2 0种有机氯农药的残留量。方法的检测限为 1 .0ng/g～ 2 0 .0ng/g ,回收率为 83.2 %～ 1 0 6.8% ,RSD为 2 .0 %～9.5%。     

毛细管气相色谱法测定5种中草药中有机氯农药的残留量

建立了怀牛夕等 5种中草药中六六六及滴滴涕异构体含量的气相色谱分析方法。样品以石油醚 +丙酮在索氏提取器中提取 ,提取液以浓硫酸净化。采用SE 30弹性石英毛细管柱分离样品 ,GC ECD检测六六六、滴滴涕农药的残留量。方法的线性范围为 5 .7× 10 - 7～ 2 .8× 10 - 4μg ;最小检测量为 1.3× 10 - 1 4～ 2 .5×10 - 1 2 g ;加样平均回收率为 88.8%～ 99.1% ;RSD为 0 .9%～ 5 .3%。     

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。     

银杏叶中18种有机氯农药的多残留分析

建立了银杏叶中18种有机氯农药残留量的气相色谱分析方法。对浓硫酸磺化法实验条件进行了优化。样品以丙酮∶石油醚(1∶1)超声提取15 m in,提取液使用含10%H2O浓H2SO4磺化净化,采用DB-1701石英毛细管柱分离样品,GC-ECD测定18种有机氯农药的残留量。此方法3个水平的加样回收率范围为71.6%~130.3%,RSD为2.2%~15.8%。方法快速简便且成本低。     

气相-质谱法测定粮谷中恶草酮的残留量

 应用微量化学法和固相萃取技术 ,建立了粮谷中恶草酮残留量的气相 质谱 (GC MS)测定方法。用苯 正己烷 (体积比为 1∶1)萃取 ,中性氧化铝小柱净化。净化液用GC MS测定 ,采用外标法定量。恶草酮在大米中的回收率为 90 4%～ 115 .7% ,RSD为 2 %～ 6 % ,在玉米中的回收率为 81 3%～ 10 9 7% ,RSD为 4%～ 9% ,最低定量检出限为 0 0 0 5mg/kg。该法快速、灵敏、准确 ,各项技术指标均满足农药残留检测的要求。     

顶空气相法测定氯乙烯生产过程产生的盐酸溶液中的乙炔和氯乙烯

 采用顶空气相法测定了氯乙烯生产过程产生的盐酸溶液中的乙炔和氯乙烯。使用氢氧化钠将试样中的氯化氢中和 ,从而消除其在气相分析乙炔和氯乙烯中的影响。顶空平衡温度为 35℃ ,平衡时间为 4 5min ,柱为填充了GDX 2 0 2固定相的 2m× 3mmi d 不锈钢柱 ,柱温 14 0℃。顶空气体进样量为 1mL。以外标法定量 ,乙炔含量测定结果的相对标准偏差为 0 85 % ;当其含量为 30 0 μg/g～ 15 0 μg/g时 ,回收率为 98 9%～10 3%。氯乙烯含量测定结果的相对标准偏差为 1 4 % ;当其含量为 2 0 0 μg/g～ 10 0 μg/g时 ,回收率为 98 8%～10 2 %。     

响应面法优化吹扫捕集结合气相色谱—串联质谱法测定消毒洗手液中10种含氧有效成分

采用吹扫捕集-气相色谱串联质谱(P&T-GC-MS/MS)技术建立了测定消毒洗手液中10种含氧消毒有效成分的方法。样品用蒸馏水稀释处理，稀释液吹扫进样，通过响应面方法优化吹扫条件，目标物通过吹扫富集于捕集阱中，热脱附后进入气相色谱。经DB-624 UI色谱柱(60 m×0.25 mm×1.40μm)分离后，采用多反应监测(MRM)模式分析检测，内标法定量。11种消毒有效成分在浓度4～250 ng/mL范围内与峰面积呈线性关系。方法定量限为0.005～0.0115μg/g,能满足相关标准中对甲醇等物质的限值要求。样品加标回收率在85.1%～116.0%,相对标准偏差(RSD)≤5.3%(n=6)。结果表明本方法快速简单、准确可靠，适用于进出口消毒洗手液中10种含氧有效成分的批量分析测定。     

固相萃取–毛细管气相色谱法同时测定水体中8种有机磷类农药残留

建立固相萃取–毛细管气相色谱法同时测定水体中敌敌畏、乙酰甲胺磷、治螟磷、乐果、甲基对硫磷、马拉硫磷、杀螟硫磷和水胺硫磷8种有机磷类农药残留。样品经OASIS HLB固相萃取柱富集,丙酮洗脱,用毛细管气相色谱(FPD)法进行定量分析。8种有机磷类农残留的质量浓度在0.05~4.0μg/m L范围内与色谱峰面积线性关系良好,相关系数均大于0.998,方法检出限为0.004~0.01μg/m L。测定结果的相对偏差为2.6%~4.5%(n=6),加标回收率为81.6%~106.2%。该方法操作简单、灵敏度高,可用于检测水体中的8种有机磷类农药残留。     

Simplified method for the determination of organochlorine pesticides in honey.

A method is described for the detection and quantitative determination of organochlorine pesticides in honey. After extraction with hexane, the pesticides were cleaned-up by adsorption chromatography on a Florisil Sep-Pak cartridge and eluted with 15% diethyl ether in hexane. The detection of organochlorine pesticides was performed by capillary gas chromatography with electron-capture detection. The quantification limit obtained for different pesticides ranged from 0.56 to 2.78 micrograms kg-1 and recoveries from fortified honey samples averaged 89.6%.     

Amperometrische Bestimmung von Pflanzenschutzmitteln in technischen Wirkstoffen und Formulierungen

Zusammenfassung Zur Bestimmung verschiedener technischer Wirkstoffe und Formulierungen von Pflanzenschutzmitteln aus der Harnstoff- und Carbamat-Gruppe wird eine Diazotitration mit amperometrischer Endpunktanzeige vorgeschlagen. Als Test-Wirkstoffe werden Monuron, Diuron, Linuron, Metoxuron, Propham, Chlorpropham und Formetanat-HCL verwandt. Die erhaltenen Ergebnisse werden mit verschiedenen dünnschicht-chromatographischen und titrimetrischen Vergleichsmethoden überprüft. Die relativen Standardabweichungen der Ergebnisse liegen bei etwa 0,5% für die Bestimmung von technischen Wirkstoffen und bei etwa 1% für die Bestimmung von Wirkstoffen in Formulierungen.

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Amperometric determination of pesticides in technical products and formulations

A diazotisation titration with amperometric indication of the end-point for determination of active ingredients and formulations of urea and carbamate pesticides has been investigated. Test materials were Monuron, Diuron, Linuron, Metoxuron, Propham, Chlorpropham and Formetanate-HCl. Results were compared with those of thin-layer Chromatographic and titrimetric methods. Relative standard deviations for determinations of active ingredients in technical products are about 0.5%, those for formulations about 1%.

     

A new method for the quantitative analysis of organochlorine pesticides and polychlorinated biphenyls

A simple method is described for the quantitative determination of organochlorine pesticides and polychlorinated biphenyls (PCB's) in water at the sub-ppb level. A micro gas-phase extractor advantageously replaces other preconcentration and purification techniques. The extract is analyzed by capillary gas chromatography without further enrichment. The recovery at the ppb level was nearly 100% for organochlorine pesticides and more than 80% for PCB's. The complete procedure including sample preparation, steam distillation-extraction, and capillary gas chromatographic analysis is carried out in less than four hours.     

毛细管胶束电动色谱分离测定大米中农药类环境激素乐果、克百威和灭多威残留

用毛细管胶束电动色谱分离测定了3种农药类环境激素乐果、克百威和灭多威在大米中的残留。考察了电泳缓冲溶液的pH值、浓度及表面活性剂浓度等影响因素,在pH=7.0的20mmol/L硼酸-四硼酸钠缓冲溶液+70mmol/L十二烷基硫酸钠(SDS)+10%甲醇体系中,三组分在16min内得到基线分离。乐果、克百威及灭多威的检测限分别为0.01、0.02和0.008mg/kg,回收率范围为101.31%～102.63%,相对标准偏差(RSD)<5%。该方法具有操作简单、快速、重现性好等优点。     

Determination of pesticide residues in lettuce by gas chromatography with electron-capture detection

A sensitive, rapid, and simple multiresidue method for the simultaneous determination of 19 pesticides in different varieties of lettuce (Lactuca sativum) was developed. Lettuce samples were extracted by homogenization with acetone and partitioned into ethyl acetate-cyclohexane. Subsequent sample cleanup was not needed. Final determination was made by capillary gas chromatography (GC) with electron-capture detection (ECD). Confirmation analysis of pesticides was performed by GC coupled with mass spectrometry in the selected ion monitoring mode. The average recovery by the GC-ECD method obtained for these compounds varied from 66.4 to 119.2% with relative standard deviations < 7.7%. The GC-ECD method has good linearity, and the detection limit for the pesticides studied varied from 0.1 to 3.8 microg/kg. The proposed method was used to determine pesticide levels in different types of lettuce grown in soils from experimental fields.     

Separation and simultaneous determination of the active ingredients in theophylline tablets by micellar electrokinetic capillary chromatography

The separation and determination of seven active ingredients in theophylline tablets by micellar electrokinetic capillary chromatography is described. On a 35 cm × 50 μm I.D. capillary, baseline separation is possible with a carrier solution containing 0.05 M sodium dodecyl sulphate (SDS) in 0.02 M borate buffer (pH 9.2) solution. The migration time of solutes increased markedly with increasing SDS concentration and slightly with increasing pH. With consecutive injections of samples, slight decreases in the migration times of the solutes occurred, but they were in parallel, owing to the temperature rise of the capillary with time. The column efficiency was influenced by the micellar concentration and applied voltage, and optimum values at which the highest theoretical plate number was achieved were established. The determination of the active ingredients was performed using hydrochlorothiazide and levamisole hydrochyloride (for ephedrine hydrochloride only) as internal standards, with good linearity with correlation coefficients from 0.9965 to 0.9999 and recoveries from 94.1 % to 101.1%. For quantitative information, measurements of peak height were better than peak area.     

中红外、近红外和拉曼光谱法测定商品农药制剂中氰戊菊酯和马拉硫磷的含量

利用近红外、中红外和拉曼光谱法定量分析了商品农药制剂中有效成分氰戊菊酯和马拉硫磷的含量.采用偏最小二乘法(Partial least squares,PLS)建立氰戊菊酯和马拉硫磷的定量模型并进行了优化,用独立检验集对模型适应性进行评价.近红外和中红外法测定氰戊菊酯、马拉硫磷定量模型的相关系数分别是0.9981,0.9994和0.9946,0.9998,外部验证集标准差分别是0.082,0081和0.092,0.075,两种方法的定量效果接近;拉曼法氰戊菊酯和马拉硫磷定量模型的相关系数分别为0.9872和0.9993,外部验证集标准差分别为0.254和0.317,预测精度不及近红外和中红外法高.MIR-ATR,NIR和Raman 3种方法均能满足现场检测农药质量的需要.     

双毛细管气相色谱法测定果蔬中有机磷及氨基甲酸酯类农药残留

对果蔬样品中残留的有机磷及氨基甲酸酯农药,通过较为简便有效的提取方法,以双毛细管柱气相色谱法进行测定,排除了干扰影响,增加了试验结果的可靠性,取得了满意结果。     

气相色谱法测定茶叶中的噻嗪酮、甲胺磷、乙酰甲胺磷及三唑磷残留

建立了同时测定茶叶中噻嗪酮、甲胺磷、乙酰甲胺磷和三唑磷4种农药残留量的测定方法。在45 ℃加温条件下,用乙酸乙酯-正己烷混合溶剂提取及活性炭色谱柱净化,用不同配比的乙酸乙酯-正己烷混合液梯度洗脱待测组分,以DB-210毛细管色谱柱分离、氮磷检测器测定。结果表明,上述4种农药在10 min内能很好地分离;样品加标回收率(n=3)为73.4%~96.9%。方法的变异系数为2.49%~3.35%,茶叶（干重）中4种农药的定量检测下限为7.0~12.0 μg/kg。