广西北部湾蔬菜种植基地土壤中代森锌类农药残留调查

采用顶空-气相色谱-质谱法,对南宁、北海、钦州和防城港等4个北部湾区域城市蔬菜种植基地60份土壤样品中的代森锌类农药残留进行检测。结果表明,南宁市的15份土壤样品均未检出代森锌类农药残留;北海市有5份土壤样品检出代森锌类农药残留,检出率为33.3%,其质量比范围为0.005 2 mg/kg~0.034 6 mg/kg;钦州和防城港2市30份土壤样品均检出代森锌类农药残留,检出率为100%,其质量比范围为0.004 9 mg/kg~0.674 mg/kg。     

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%。     

微库仑法和离子色谱法测定土壤中可吸附有机卤素

采用振荡吸附处理土壤样品，用微库仑法和离子色谱法分别测定土壤中的可吸附有机卤素(AOX)。通过优化样品前处理条件以提高AOX的提取效率，上述两种方法检出限分别为15.3 mg/kg和16.3 mg/kg, 4-氯苯酚作为标准物质的加标回收率分别为92.2%～95.0%和77.7%～80.2%。两种方法测定实际土壤样品中AOX,6次测定结果的RSD为5.4%～19.2%。GSS系列标准土壤试验结果表明，振荡吸附处理样品，用微库仑法和离子色谱法在测定样品中AOX时测定结果区别不大，土壤中AOX含量与卤素含量无直接关系。     

贵州省部分地区土壤中酞酸酯类污染现状调查

对贵州省部分地区表层土壤中酞酸酯类的污染状况进行了调查。分别在遵义地区、黔南地区、黔东南地区和毕节地区采集483个土壤样品分析,结果表明,样品中酞酸酯总质量比(ΣPAEs)为未检出~8.22 mg/kg,均值为0.63 mg/kg。其中DEHP和DBP为主要污染物,均值分别为0.32 mg/kg和0.24 mg/kg,检出率分别为90.89%和97.10%。     

高效液相色谱法测定柑橘及橘园土壤中乙撑硫脲残留

建立了高效液相色谱测定柑橘及橘园土壤中乙撑硫脲残留的方法,优化了试验条件.方法在0 mg/L～5.35 mg/L范围内线性良好,橘园土壤、橘皮、橘肉样品的检出限(以鲜重计)分别为0.006 mg/kg、0.008 mg/kg、0.006 mg/kg,样品测定的RSD≤5.1%,加标回收率为82.9%～92.8%.     

开氏消煮-常量蒸馏-滴定法测定土壤中总氮量

文章对开氏消煮-常量蒸馏-滴定法测定总氮过程中样品消解时间和消解温度对样品测定值的影响及测定方法进行了研究。测定了不同含氮量的土壤样品,样品相对标准偏差为1.6%-3.9%,与经典法测定相比相对偏差为0.2%-3.1%。认为该方法适用于土壤总氮的测定,与经典法相比操作简便,适用大量样品的检测。     

气相色谱法同时测定稻田中稻瘟酰胺和咪鲜胺残留

采用二氯甲烷萃取稻田水样品,土壤样品用丙酮-二氯甲烷(体积比为9∶1)混合溶液提取,二氯甲烷萃取,水稻植株样品用乙腈-二氯甲烷(体积比为9∶1)混合溶液直接萃取,用气相色谱法同时测定样品中稻瘟酰胺和咪鲜胺残留。该方法在0.012 2 mg/L~2.68 mg/L范围内线性良好,稻田土壤、田水、水稻植株中稻瘟酰胺的检出限分别为2.75μg/kg、1.83μg/L、3.80μg/kg,咪鲜胺的检出限分别为3.55μg/kg、2.66μg/L、5.62μg/kg。空白稻田土壤、稻田水和水稻植株样品3个浓度水平的加标回收率为80.3%~104%,RSD为3.0%~13.2%。     

污染土壤中六价铬的测定

通过加入碱性消解液、MgCl2和磷酸缓冲溶液,建立了污染土壤中六价铬的分光光度测定法.方法在0 mg/L～0.200 mg/L范围内线性良好,检出限为0.16 mg/kg(以2.5 g样品计),土壤样品测定的RSD为4.6%,加标回收率为92.3%～107%.     

超声波萃取-红外分光光度法测定土壤中石油类

采用超声波萃取-红外分光光度法测定土壤中石油类,并对超声波机的功率、水浴温度和萃取时间进行优化.试验表明：方法在0mg/L～80.0mg/L范围内线性良好,相关系数r为0.9997;方法检出限为6.00μg/L,当取土壤样品10.0g时,方法检出限为0.03mg/kg;空白土壤的加标回收率为97.4% ～103%;测定实际土壤样品的RSD为3.0% ～3.9%.通过比较超声波萃取、四氯化碳热浸法和快速溶剂萃取法的前处理效果,显示出超声波萃取法的优越性.     

加压溶剂萃取/气相色谱-质谱法测定土壤中的三嗪类农药

建立了加压溶剂萃取/气相色谱-质谱法,用于测定土壤中的10种三嗪类农药。以正己烷-丙酮(体积比1∶1)为萃取剂,对土壤样品进行加压溶剂萃取。将提取液净化浓缩后,采用气相色谱-质谱联用仪进行检测,根据保留时间和特征离子定性,内标法定量。10种三嗪类农药在0.05～5 mg/L范围内的线性关系良好(相关系数≥0.997),检出限为0.002～0.003 mg/kg。对实际土壤样品进行高、中、低浓度加标,测得的回收率范围为66.7%～102%,相对标准偏差范围为0.79%～5.49%。该方法简便可靠、灵敏度高,适用于土壤中三嗪类农药的测定。     

G C/MS法测定环境空气中痕量POPs类有机氯农药及降解产物

采用快速溶剂萃取-氟罗里硅土柱净化-气相色谱/质谱联用法测定环境空气中POPs类有机氯农药及其降解产物.艾氏剂、狄氏剂、异狄氏剂、六六六、滴滴涕,七氯、氯丹、灭蚁灵及其降解产物的检出限为2.0 ng～4.6 ng,空白加标回收率为62.1%～118%,RSD为6.8%～15.2%.     

Pesticide Residues in Bovine Milk from a Predominantly Agricultural State of Haryana, India

One hundred forty seven samples of bovine milk were collected from 14 districts of Haryana, India during December 1998–February 1999 and analysed for the presence of organochlorine pesticide (OCPs) residues. ∑HCH, ∑DDT, ∑endosulfan and aldrin were detected in 100%, 97%, 43% and 12% samples and with mean values of 0.0292, 0.0367, 0.0022 and 0.0036 μg/ml, respectively. Eight percent samples exceeded the maximum residue limit (MRL) of 0.10 mg/kg as recommended by WHO for ∑HCH, 4% samples of 0.05 mg/kg for α-HCH, 5% samples of 0.01 mg/kg for γ-HCH, 26% samples of 0.02 mg/kg for β-HCH as recommended by PFAA and 24% samples of 0.05 mg/kg as recommended by FAO for ∑DDT. Concentrations of β-HCH and p,p′-DDE were more as compared to other isomers and metabolites of HCH and DDT.     

固相萃取- GC/MS法测定水中有机氯农药

建立了固相萃取-气相色谱／质谱联用测定水中痕量六六六、滴滴涕和环氧七氯的方法。采用C18固相萃取柱富集水样，二氯甲烷／丙酮混合溶剂洗脱，加入菲-d10作为内标，利用气相色谱／质谱联用仪选择离子监测模式检测，内标法定量，定性、定量准确，线性响应良好，干扰小，按采样1 L计算，方法检出限为4．26ng／L～19、2ng／L，RSD在0、4％-6、3％之间，平均加标回收率在77．7％～118％之间，实际样品测定结果表明方法能满足环境水体中痕量有机氯农药的监测要求。     

镇江地区土壤中有机氯农药残留状况研究

2006年11月采集了镇江地区69个土壤表层样品，利用ASE萃取后使用GC（ECD）法测定样品中的BHC和滴滴涕的含量。结果表明，镇江地区土壤中的BHC的检出率不高，但是滴滴涕的检出率比较高；冲积平原的检出率高于林地和滩涂；蔬菜和水稻种植区域的污染比草地、灌木丛和林地严重。     

气相色谱法测定鱼组织中的久效磷

采用气相色谱法氮磷检测器测定鱼肉和内脏中的久效磷含量。鱼肉或内脏匀浆后，用正己烷洗涤，二氯甲烷提了，以内标法定量分析，方法简单，灵敏，准确。当取鱼组织0．5g时，方法检测限为0．002mg/kg，加标回收率为72．6％－83．3％，相对标准差在3．3％－7．0％之间。     

胭脂红酸分光光度法测定废水中硼

用胭脂红酸分光光度法测定废水中的硼，着重进行了方法的条件和干扰试验。方法检测限为0.063mg/L，线性范围为0.21mg/L-1.25mg/L。5个实验室对5.00mg/L硼标准样品测得重复性相对标准差为3．4％，再次性相对标准差为3．6％；相对误差为－0．8％－1．4％，回收率在95．2％－104．6％之间。     

气相色谱法测定环境空气中氯化苄和甲苯

用串联的乙醇吸收管收集环境空气中的氯化苄和甲苯，以毛细管柱分离，氢火焰检测器测定，保留时间定性，峰高定量。氯化苄平均浓度在４．２９ｍｇ／Ｌ～２１．４ｍｇ／Ｌ时，相对标准偏差在３．３％～４．６％之间；甲苯平均浓度为４．１８ｍｇ／Ｌ～２０．６ｍｇ／Ｌ时，相对标准差在４．４％～７．８％范围内。方法快速、灵敏度高，有较好的精密度与准确度。     

Assessment of the levels of DDT and DDE in soil and blood samples from Tabasco, Mexico

In Mexico, 1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane (DDT) was used until the year 2000, principally in agriculture and anti-paludal program health campaigns. The southeastern region of Mexico was an important area of malaria, and from 1957 DDT was applied indoors every 6?months, with a coverage of 2?g/m². The current study was performed in Tabasco, a Mexican state located in the southeastern region of Mexico. DDT and 1,1-dichloro-2,2-bis(4-chlorophenyl)ethene (DDE) were analyzed by gas chromatography/mass spectrometry. In general, low levels were found in household outdoor samples; the levels of DDT ranged from not detectable to 0.048?mg/kg, and of DDE from 0.001 to 0.068?mg/kg. An important finding was that, in all communities where DDT in blood was analyzed, exposure to DDT was found, indicating both past and present exposure. Although the levels found in this study were lower than other studies in Mexico, there is a need to evaluate whether the people living in the study area are at risk.     

Environmental and Biological Monitoring of Organochlorine Residues after the Plague Epidemic in Surat, India - A Preliminary Study

In late August 1994, an outbreak of human pneumonic/bubonic plague was reported in Surat, India. During the epidemic, large amounts of pesticides, such as benzene-hexachloride (BHC) and other organochlorinated compounds were used to control the vector that might have transmitted the plague. In order to evaluate the extent of contamination, both environmental samples (9 water samples and 4 soil samples) and biological samples (5 blood and urine samples) were collected and analyzed for organochlorine residues. Samples were analyzed after hexane extraction by gas chromatography equipped with electron capture detector (GC-ECD), using a PTE-5 capillary column. The results showed that the levels of 1,1-(2,2-dichloroethenylidene)-bis[4-chlorobenzene] (DDE), a major metabolite of DDT, were low in environmental samples (water, soil), while BHC levels were relatively high in one of the water sample as well as two soil samples. The BHC and DDE levels in the biological samples were not higher than those reported earlier from India, except for serum DDE. Further studies are needed to evaluate the effect of long-term exposure as the present study was based on limited samples.     

气相色谱法测定空气中三氯乙烯和四氯乙烯

应用气相色谱法以５％ＰＥＧ－６０００为固定液、６２０１为担体填充柱分离，电子捕获检测器检测，直接进样测定环境空气中三氯乙烯和四氯乙烯。对０．０２９ｍｇ／ｍ＾３四氯乙烯标准样作重复５次测定，其相对标准差分别为５．７％和１．５％，并在实际样品中进行加标回收试验，回收率三氯乙烯在９０％～１１０％、四氯乙烯在９４％～１０８％之间。检测限分别为０．００６ｍｇ／ｍ＾３和０．０００５ｍｇ／ｍ＾３，完全能满足环境