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1.
初丽伟  阎吉昌  陈丹  侯志广  范志先 《分析化学》2006,34(10):1482-1486
建立了生晒参、全须生晒参中19种有机氯农药残留的毛细管气相色谱分析方法。对样品中六六六的4种异构体、滴滴涕的5种异构体、四氯苯胺、六氯苯、五氯硝基苯、七氯、五氯苯胺、艾氏剂、百菌清、环氧七氯、狄氏剂及异狄氏剂共19种有机氯农药的残留量进行了测定。以石油醚-丙酮混合物作为提取剂,样品采用索氏提取,提取液用弗罗里硅土柱层析净化。采用OV-1701石英毛细管气相色谱柱分离样品,ECD检测器进行检测。在3个水平添加时的回收率(n=5)分别为75.7%~96.1%、78.8%~111.6%和81.7%~115·2%;相对标准偏差分别为2.4%~10.6%、2.1%~9.8%和1.4~10.0%。方法用于生晒参和全须生晒参样品中农药残留的测定,结果满意。  相似文献   

2.
建立了枇杷花中有机氯类农药残留量的固相萃取-毛细管气相色谱(SPE-CGC)分析方法。对采自福建蒲田等12地的枇杷花中六六六(4种异构体)、滴滴涕(4种异构体)、五氯硝基苯共9种有机氯农药的残留量进行了测定。样品采用丙酮超声波提取,浓缩后过Florisil固相萃取小柱净化,洗脱剂为V(正己烷)∶V(丙酮)100∶1。用DB-1701弹性石英毛细管气相色谱柱分离样品,微电子捕获检测器进行检测。9种有机氯农药的峰面积与其质量浓度均有良好的线性关系,相关系数均大于0.999,最低检测限为0.016~0.125μg/L,样品的加标回收率为85.4%~106.9%,相对标准偏差为1.8%~9.8%。该方法能够满足农药残留检测的要求。  相似文献   

3.
搅拌棒吸附子萃取与GC-MS法测定水中20种有机氯农药   总被引:2,自引:0,他引:2  
建立了搅拌棒吸附子萃取/气相色谱-质谱法(SBSE/GC-MS)同时检测水中α-六六六、γ-六六六、β-六六六、七氯、δ-六六六、艾氏剂、环氧七氯、γ-氯丹、顺-氯丹、硫丹Ⅰ、p,p-滴滴伊、狄氏剂、异狄氏剂、p,p-滴滴滴、硫丹Ⅱ、p,p-滴滴涕、异狄氏剂醛、硫丹硫酸盐、甲氧滴滴涕、异狄氏剂酮20种有机氯农药含量的方法.样品在室温下经拌棒吸附子搅拌吸附,甲醇解吸附后,以J&W DB-35 MS(30 m×0.25 mm×0.25 μm)石英毛细管色谱柱为分析柱,气相色谱-质谱选择离子流模式检测.考察了萃取时间、氯化钠及甲醇加入量等对萃取的影响.实验结果表明:在2.5 ~20.0 μg/L 范围内,20种有机氯农药呈良好的线性关系,检出限(S/N=3)为0.008 ~0.118 μg/L,水样中分别添加2.5、20 μg/L的20种有机氯农药,回收率为 52% ~117%,相对标准偏差小于13%(n= 6).该方法操作简便、快速、灵敏度高,应用于实际样品检测,结果满意.  相似文献   

4.
建立了中草药及其土壤中多种有机氯农药残留量的固相萃取-毛细管气相色谱(SPE-CGC)分析方法,并对7种中草药及其土壤中多种有机氯农药残留量的相关性进行了初步研究。样品以正己烷-丙酮用超声波提取,Florisil(1 g)固相萃取小柱快速净化提取物。采用SPB-5弹性石英毛细管柱分离样品,GC-ECD检测7种中草药及其土壤中的13种有机氯农药的残留量。方法的线性范围为1.26×10-10~2.24×10-7g/mL;检出限为6.4×10-11~6.1×10-10g/mL;加样平均回收率为87.3%~104.4%(RSD为1.1%~7.0%)。  相似文献   

5.
建立了加速溶剂提取、固相萃取净化、气相色谱-离子阱串联质谱法测定土壤和沉积物中25种有机氯农药和多氯联苯单体的分析方法.六六六、滴滴涕等17种有机氯农药(OCPs)的方法检出限(MDL)为0.049~0.274μg/kg,除异狄氏剂(线性范围为3.45~441.6μg/L)外,其余16种OCPs的线性范围均为1.73~...  相似文献   

6.
建立了毛细管气相色谱法检测桑叶中农药多残留的方法。样品以乙腈为提取剂,提取液用弗罗里硅土柱净化,乙酸乙酯∶正己烷(体积比15∶85)洗脱,采用HP-5与DB1701毛细管色谱柱双柱,气相色谱-电子捕获检测法(GC-ECD)测定42种有机氯及拟除虫菊酯类农药及其异构体的残留量。结果表明:该方法在20、80、160μg/kg 3个添加水平下回收率分别为78.6%~110.3%、78.3%~109.6%、80.1%~109.1%,相对标准偏差(RSD)均在1.1%~11.3%,符合农药残留分析的要求。该方法重复性及净化效果好,可用于桑叶中42种有机氯及拟除虫菊酯类农药及其异构体的残留量检测。  相似文献   

7.
采用分散固相萃取(Dispersive solid-phase extraction)样品前处理方法,建立了蕨菜、黑米等生态农产品中53种农药残留的气相色谱一质谱(GC-EI/MS)的分析方法.样品由含0.1%冰醋酸的乙腈提取,以环氧七氯为内标,经分散固相萃取法净化.每种农药选择了合适的离子及其驻留时间,采用气相色谱-...  相似文献   

8.
建立了一种固相萃取/气相色谱-质谱法同时测定土壤中23种有机氯农药的方法,并研究了不同基质效应补偿方式。土壤样品经正己烷∶丙酮(体积比1∶1)提取,弗罗里土小柱净化,采用气相色谱-质谱仪检测。结果发现7种有机氯存在中/强程度的基质效应;在10 mL二氯甲烷∶正己烷(体积比1∶9)+10 mL丙酮∶正己烷(体积比1∶9)为固相萃取的洗脱剂,且脉冲压力为275.8 kPa条件下,可将23种有机氯的基质效应均控制在20%以内。23种有机氯农药在0.4~10μg·mL~(-1)质量浓度范围内线性良好,相关系数(r~2)均不小于0.999 2,检出限为1.0~8.6μg·kg~(-1),定量下限为4.0~34.4μg·kg~(-1);在20、60、100μg·kg~(-1)3个加标水平下空白土壤中的平均回收率为46.3%~127%,相对标准偏差(n=6)为0.68%~15%。采用该方法在某土壤样品中检出α-六六六、γ-六六六、p,p′-DDE、异狄氏剂醛、p,p′-DDT 5种有机氯农药。  相似文献   

9.
毛细管气相色谱法测定清补凉中六六六、DDT的残留量   总被引:1,自引:0,他引:1  
建立毛细管气相色谱法测定清补凉中六六六、滴滴涕(DDT)的残留量。用丙酮提取样品中残留的有机氯农药,石油醚萃取,萃取液以浓硫酸净化。采用HP-1石英毛细管色谱柱对清补凉中8种六六六、DDT的异构体进行了检测。结果表明,该法测定下限为2.45×10-14~1.15×10-12g,加标平均回收率为84.9%~98.6%,相对标准偏差为1.6%~4.5%。  相似文献   

10.
微波辅助萃取法测定烟草中有机氯类农药残留量   总被引:5,自引:0,他引:5  
建立了一种微波辅助萃取-固相萃取净化测定烟草中17种有机氯类农药残留量的新方法. 样品用V(正己烷):V(乙酸乙酯)=1:1提取, 提取液经Florisil固相萃取柱净化后, 采用气相色谱-电子捕获检测器(GC-μECD)进行检测. 17种有机氯农药的0.01、 0.05 mg/kg和0.5 mg/kg加标回收率均在82%以上, RSD在0.11%~8.2%之间, 能满足当前烟草中有机氯农药残留的检测要求.  相似文献   

11.
A method for the determination of trace levels of triazines and organophosphorus pesticides in water is presented. The extraction method is based on a solid-phase extraction on C-18 bound silica SPE cartridges. A precolumn filled with Merck C-18 bound silica and home-made C-18 bound silica have been tested at a flow-rate of 3 ml/min with comparable preconcentration yields. A SIM-MS method using a (15)N labelled internal standard has been developed for the organophosphorus pesticides. Detection limits lower than 1 microg/L have been obtained. Separations have been carried out on a conventional GC column OV 17 (1 m) and a capillary column OV 17 (25 m) with a temperature program from 150 degrees C (2 min) to 300 degrees C (rate of 6 degrees C/min).  相似文献   

12.
牟峻  陈明岩  邹明强 《色谱》1999,17(4):386-388
 介绍应用气相色谱-质谱法测定纺织品、皮革及其制品中防霉剂五氯苯酚的残留量,试样经硫酸溶液酸化后用正己烷提取,用气相色谱-质谱选择离子测定。方法简便、快速、灵敏,检出限20μg/kg,添加回收率86.7%~93.1%,变异系数4.1%~5.9%。  相似文献   

13.
固相微萃取-气相色谱/质谱分析栀子花的头香成分   总被引:30,自引:0,他引:30  
刘百战  高芸 《色谱》2000,18(5):452-455
 分别用固相微萃取和动态顶空法分离栀子鲜花的头香成分,用GC/MS技术分析鉴定,并用GC/MS总离子流色谱峰的峰面积进行归一化定量。在固相微萃取方法中,共鉴定了54种化学成分,占总峰面积的99.98%。主要成分(质量分数)依次为金合欢烯(64.86%)、罗勒烯(29.33%)、芳樟醇(2.74%)、惕各酸顺式叶醇酯(1.34%)和苯甲酸甲酯(0.25%)等。经与动态顶空法的分析结果比较发现,固相微萃取法不仅操作简便,而且具有较高的采样灵敏度,获得的化学成分的信息量多于动态顶空法。  相似文献   

14.
A procedure is developed for the simultaneous determination of polychlorinated biphenyls and organochlorine pesticides in fish and fish products by gas-liquid chromatography with an electron capture detector on a capillary column DB-1701 (30 m × 0.25 mm × 0.25 μm) under temperature-programming conditions. The detection limit is 0.06 μg/kg of the test sample. Polychlorinated biphenyls and organochlorine pesticides were extracted from the samples using a hexane-acetone mixture (1 : 1). Lipids were removed by treatment with H2SO4. Eighteen samples were analyzed; the concentrations of pollutants were found to be below the prescribed values.  相似文献   

15.
A headspace solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to flame ionization detector (GC-FID) is developed for the direct determination of volatile fatty acids (VFAs) in wastewater from constructed wetlands. Through the investigation on extraction behavior of different coatings for VFAs and the chromatographic behavior of VFAs in a Stabilwax-DA capillary column (30 mx0.32 mm i.d., 0.25 microm film thickness) using nitrogen as carrier gas, the polyacrylate fiber is selected as the satisfactory coating for VFAs analysis, and optimum chromatographic conditions are obtained. The oven temperature is programmed at 70 degrees C for 2 min, then a 4 degrees C/min rate until 180 degrees C, holding 2 min, and then a 20 degrees C/min rate until 200 degrees C, holding the final temperature for 3 min. The various parameters including extraction time, extraction temperature, pH value, ion strength, sample volume, and desorption conditions are investigated for the optimization of HS-SPME performance for VFAs in the wastewater. The experimental results show that the linear dynamic ranges are 10-45000 microg/L, and over two to four orders of magnitude depending on different acids. The detection limit (3sigma) for VFAs are low to microg/L levels and the relative standard deviations are less than 10%, and the recoveries are between 85% and 117%. By using 2-ethylbutyric acid as internal standard, the proposed method is successfully applied to the determination of VFAs in wastewater from the constructed wetlands.  相似文献   

16.
A method involving the simultaneous extraction and separation of 12 organochlorine pesticides (OCPs) from Angelicae sinensis was developed using supercritical fluid extraction (SFE). The pesticides in the study were alpha-, beta-, gamma- and delta-benzene hexachloride, PCNB (pentachloro- nitrobenzene), PCA (pentachloroaniline), HEPT (heptachlor), MPCPS (methyl-pentachlorophenyl sulfide), pp'-DDE [1,1-dichloro-2,2-bis (p-chlorophenyl) ethylene], op'-DDT [1,1,1,-trichloro-2-(o-chlorophenyl)-2-(p-chlorophenyl) ethane], pp'-DDD [1,1-dichloro-2,2-bis(p-chlorophenyl) ethane], and pp'-DDT [1,1,1,-trichloro-2,2-bis (p-chlorophenyl)ethane]. The extraction conditions were optimized as follows: pure CO(2), extraction pressure 15 MPa, extraction temperature 60 degrees C, extraction time 20 min, and flow-rate 1.5 mL/min. A GC method with electron capture detection was employed to determine the OCPs in Angelicae sinensis. An HPLC method was developed for the quantitative determination of active constituents. The SFE provided high decontamination rate of OCPs and low loss of active constituents in Angelicae sinensis.  相似文献   

17.
A method involving depuration of 12 organochlorine pesticides (OCPs) from Radix codonopsis was developed using supercritical fluid extraction (SFE). The pesticides investigated in the study included alpha-, beta-, gamma- and delta-benzene hexachloride, PCNB (pentachloro-nitrobenzene), PCA (pentachloroaniline), HEPT (heptachlor), MPCPS (methyl-pentachlorophenyl sulfide), pp'-DDE [1,1-dichloro-2, 2-bis(p-chlorophenyl) ethylene], op'-DDT [1,1,1-trichloro-2-(o-chlorophenyl)-2-(p-chlorophenyl)ethane], pp'-DDD [1,1-dichloro-2-2-bis(p-chlorophenyl)ethane] and pp'-DDT [1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane]. A series of experiments was conducted to optimize the final extraction conditions as follows: pure CO2, extraction pressure 15 MPa, extraction temperature 60 degrees C, extraction time 20 min and flow rate 55 mL/h. A GC method with electron capture detection was employed for the determination of the OCPs in Radix codonopsis. An HPLC method was developed for the quantitative determination of active constituents. SFE was used to remove the organochlorine pesticide from Radix codonopsis. The results showed that at least 93.5% of the organochlorine pesticide residues in the herb sample were removed by SPE, while 95.0% of the active constituent marker (atractylenoide III) remained.  相似文献   

18.
气相色谱-质谱法分析橡苔浸膏中的挥发性化学成分   总被引:1,自引:1,他引:0  
高芸  刘百战  朱晓兰  时亮  陈加林  宫梅  张龙根 《色谱》2000,18(3):251-253
 用挥发油提取器提取橡苔浸膏中的挥发油,利用气相色谱-质谱法(GC-MS)分析了其中的化学成分,采用GC峰面积归一化法定量,鉴定出24种化合物,共占挥发油总量的83%以上  相似文献   

19.
气相色谱法直接测定植物生长素   总被引:12,自引:0,他引:12  
杜黎明  许庆琴 《色谱》2000,18(2):160-161
 建立了一种采用 5 3 0 μm大口径毛细管色谱柱、不经衍生化处理而直接测定吲哚乙酸 (IAA)、吲哚丁酸(IBA)和萘乙酸 (NAA)等植物生长素的气相色谱分析方法。以邻苯二甲酸二丁酯为内标物 ,用 FID检测 ,IAA,IBA和 NAA的相对标准偏差分别为 1 .1 4% ,0 .61 %和 0 .78%。方法简便、快速、准确、重现性好 ,可用于生长素类单组分和混合制剂的质量检测。  相似文献   

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