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1.
血浆中有机磷农药的固相萃取—气相色谱法测定   总被引:4,自引:0,他引:4  
建立了固相萃取,GC-FPD(火焰光度检测器)测定血浆中有机磷农药含量的方法,血样经固相萃取,GC-FPD分析,杂质干扰少,血中有机磷农药提取回收率在74%以上,RSD在7.8%-20%,检出限,敌敌畏,乐果为10ug/L,甲拌磷,对硫磷为5ug/L,经实际中毒病人样品分析,证明该法操作简便,准确可靠,灵敏度高。  相似文献   

2.
毛细管气相色谱法测定中药中有机磷农药残留量   总被引:9,自引:0,他引:9  
建立了中药中多种有机磷农药残留量的毛细管气相色谱测定方法。样品以丙酮-石油醚混合溶剂为提取剂,超声提取后,用固相吸附层析柱(装填4g弗罗里硅土和2g中性氧化铝)净化,采用GC—FPD法同时测定中药中多种有机磷农药残留量。方法检出限为0.011~0.015μg/mL,回收率为85.5%~107.8%。该法简便、准确,能满足实际样品分析。  相似文献   

3.
建立了微波辅助萃取–气相色谱法测定茶叶中甲胺磷、乐果、毒死蜱、水胺硫磷、三唑磷5种有机磷农药残留量的分析方法。样品用乙酸乙酯微波辅助提取,提取液经分散固相萃取法(DSPE)净化,用气相色谱配FPD检测器测定,外标法定量。结果表明农药混合标准溶液在0.01~0.5μg/mL范围内线性良好(r>0.999),方法的检出限为0.005~0.01 mg/L,在0.05,0.125,0.5μg/mL 3个水平添加平均回收率为63.3%~99.9%,测定结果的相对标准偏差为5.1%~8.2%(n=6)。该方法适合于茶叶中多种有机磷农药残留量的同时检测。  相似文献   

4.
建立了高效溶剂萃取(HPSE)-固相萃取(SPE)/气相色谱-质谱(GC-MS)测定大气颗粒物中16种多环芳烃(PAHs)和15种有机磷阻燃剂(OPFRs)的方法。以正己烷-二氯甲烷(1∶1,体积比)溶液为萃取溶剂,萃取液旋转蒸发浓缩后经Florisil固相萃取柱净化,PAHs和OPFRs的洗脱溶剂分别为10 mL正己烷-二氯甲烷(1∶1)和10 mL乙酸乙酯,洗脱液浓缩定容后进行GC-MS测定。16种PAHs和15种OPFRs的线性范围为0.001 ~ 2.0 μg/mL,相关系数(r2)均大于0.99;检出限(LOD,S/N = 3)分别为0.10 ~ 10.00 μg/L和2.59 ~ 75.00 μg/L,定量下限(LOQ,S/N = 10)分别为0.33 ~ 33.33 μg/L和8.63 ~ 250.00 μg/L;平均回收率分别为73.0% ~ 98.0%和69.3% ~ 111%,相对标准偏差(RSD)分别为3.7% ~ 13%和2.5% ~ 17%。该方法适用于大气颗粒物样品中多环芳烃和有机磷阻燃剂的测定。  相似文献   

5.
水中重点有机磷农药的毛细管气相色谱法测定   总被引:11,自引:0,他引:11  
研究建立了气相色谱-火焰光度检测器(GC-FPD)法测定水中14种有机磷农药的分析方法,在选定的色谱条件下,14种有机磷农药在18min内得以很好的分离。在该方法下,14种有机磷农药的精密度良好,其中12种有机磷农药的加标回收率为92%-114.6%。  相似文献   

6.
黄倩  何蔓  陈贝贝  胡斌 《色谱》2014,32(10):1131-1137
制备了苯乙烯(St)和甲基丙烯酸(MAA)共聚物改性的磁性微球Fe3O4@P(St-co-MAA),并将其作为磁固相萃取吸附剂,建立了磁固相萃取(MSPE)-气相色谱(GC)-火焰光度检测(FPD)联用分析有机磷农药(OPPs)残留的新方法。以5种有机磷农药(二嗪农、甲基毒死蜱、杀螟硫磷、毒死蜱和喹硫磷)为目标分析物,考察并优化了吸附和解吸条件,确定了最佳实验条件。在最优的实验条件下,方法对5种OPPs的检出限(S/N=3)为0.013~0.305μg/L,方法的相对标准偏差(RSD,n=7)为3.1%~8.8%,富集倍数为406~951,线性范围达3个数量级。将该方法应用于新鲜番茄汁、草莓汁样品中的OPPs残留分析,加标回收率为85.4%~118.9%。该方法具有检出限低、分析速度快、富集倍数高等优点,为有机磷农药的残留分析提供了新的技术平台。  相似文献   

7.
利用顶空固相微萃取与气相色谱联用技术(HS-SPME-GC)以富勒烯聚二甲基硅氧烷(PSO-C60)固定相处制萃取头分析了塑料浸取液中的邻苯二甲酸二(2-乙基)己酯(DEHP),并对萃取温度、离子强度、吸附时间和热解析时间进行了研究。结果显示,该方法的线性范围在5μg/L-500μg/L,检测出了为2.8μg/L,相对标准偏差为4.8%(n=6).  相似文献   

8.
建立固相萃取–气相色谱同时测定水果中敌敌畏、乙酰甲胺磷、二嗪磷、治螟磷、乐果、甲基对硫磷6种有机磷农药残留的分析方法。样品均质后用乙腈进行提取,氯化钠盐析,SPE柱净化,用火焰光度检测器(FPD)进行测定,外标法定量。6种有机磷农药的线性范围为0.01~2.0μg/m L,线性相关系数不低于0.99,检出限为0.001~0.004mg/kg,测定结果的相对标准偏差均小于5%(n=6),加标回收率均在82.8%~100.0%之间。该法前处理操作简单,快速,可满足水果中多种有机磷农药残留同时分析的要求。  相似文献   

9.
固相微萃取-气相色谱法测定红葡萄酒中残留的有机磷农药   总被引:22,自引:0,他引:22  
胡媛  刘文民  周艳明  关亚风 《色谱》2006,24(3):290-293
采用溶胶-凝胶包埋技术制备了耐高温固相微萃取头(SPME),用该萃取头与气相色谱-热离子化检测器联用对红葡萄酒中的12种有机磷农药残留进行了测定。实验中对搅拌速度、萃取时间、盐浓度等条件进行了优化。结果表明,在样品用量25 mL,搅拌速度1250 r/min,盐浓度 150 g/L,萃取时间30 min的条件下,绝大多数组分峰面积的相对标准偏差(RSD)在5%以下,各种有机磷农药的检测限为5 ng/L到0.38 μg/L。  相似文献   

10.
新型固相微萃取探头测定工业废水中的甲苯和二甲苯   总被引:9,自引:0,他引:9  
采用溶胶-凝胶方法研制的聚甲基苯基乙烯基硅氧烷/羟基硅油复合涂层的固相微萃取探头及顶空固相微萃取-气相色谱联用技术(HS-SPME-GC),测定了制漆厂排放的工业废水中的甲苯和二甲苯。研究了影响该方法分析灵敏度的各种条件因素:萃取时间和温度,解吸时间和温度及离子强度等。结果表明新探头性能优于商用聚二甲基硅氧烷探头。方法的检出限为0.01μg/L-0.1μg/L,相对标准偏差小于6%;除苯以外线性范围达3个数量级。  相似文献   

11.
气相色谱-火焰光度法测定土壤中有机磷农药残留   总被引:1,自引:0,他引:1  
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。  相似文献   

12.
大葱中25种有机磷农药多残留的微波净化-气相色谱测定   总被引:4,自引:0,他引:4  
姜俊  李安  李海燕  佟克兴  周丽丽  周慧敏  赵彤 《色谱》2007,25(3):395-398
采用微波净化去除大葱中硫醚干扰、气相色谱-火焰光度检测(GC-FPD)实现了大葱基质中25种有机磷农药多残留的快速检测。25种有机磷的加标回收率为85.2%~119.6%,相对标准偏差为2.1%~14.8%。大多数农药在0.1~5.0 mg/L范围内线性关系良好,相关系数不低于0.9910,检出限为0.025~0.200 mg/L。  相似文献   

13.
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。  相似文献   

14.
In this study, γ‐Fe2O3/chitosan magnetic microspheres were synthesized and evaluated by X‐ray diffraction, SEM, thermogravimetric analysis, and static and kinetic adsorption experiments. Results showed that the magnetic microspheres exhibited good adsorption ability, and offered fast kinetics for the adsorption of trichlorfon, methamidophos, malathion, methyl parathion, dimethoate, omethoate, phosphamidon, phorate, isocarbophos, and chlorpyrifos. Based on magnetic separation, a simple method of magnetic SPE coupled to GC for the simultaneous determination of ten trace organophosphate pesticide residues was developed. Under the optimal conditions, the enrichment factor for ten organophosphorus pesticides was 10.1–364.7 and linear range was 0.001–10.0 mg/L. The LOD (S/N = 3) of the method for the ten pesticides was 0.31–3.59 μg/kg. The RSD for three replicate extractions of spiked samples was between 2.5 and 6.3%. The pear and apple samples spiked with ten organophosphate pesticides at 20 and 200 μg/kg levels were extracted and determined by this method with good recoveries ranging from 79.9 to 98.7%. Moreover, the method has been successfully applied for the determination of the ten organophosphate pesticide residues in peach samples.  相似文献   

15.
This article described a new method for the sensitive determination of organophosphorus pesticides in water samples using SPE in combination with GC‐flame photometric detection. In the procedure of method development, TiO2 nanotubes were used as SPE adsorbents for the enrichment of organophosphorus pesticides from water samples. Several factors, such as eluent and its volume, sample pH, sample volume, sample flow rate, and concentration of humic acid, were optimized. Under the optimal conditions, the proposed method had good linear ranges as 0.1–40 μg/L for each of them, LOD of 0.11, 0.014, and 0.0025 μg/L, and LOQs of 0.37, 0.047, and 0.0083 μg/L for chlorpyrifos, phorate, and methyl parathion, respectively. The proposed method was validated with real environmental water samples and the spiked recoveries were over the range of 86.5–115.1%. All these results indicated that TiO2 nanotubes, as a new SPE adsorbent, would be used widespread for the preconcentraiton and determination of environmental pollutants in the future.  相似文献   

16.
建立饮用水中微囊藻毒素(MC–RR,MC–LR)的超高效液相色谱–串联质谱检测方法。样品经PVDF针式过滤头过滤后直接进样,采用喷雾正离子源(ESI~+)和多重反应监测模式(MRM)测定。MC–RR的质量浓度在0.02~10.00μg/L范围内与色谱峰面积呈良好的线性,线性相关系数r~2=0.998 9,检出限为0.096μg/L,测定结果的相对标准偏差为6.6%~9.1%(n=7),加标回收率为99.0%~103.0%。MC–LR的质量浓度在0.1~20μg/L范围内与色谱峰面积呈良好的线性,线性相关系数r~2=0.999 2,检出限为0.188μg/L,测定结果的相对标准偏差为4.3%~10.0%(n=7),加标回收率为93.0%~114.0%。该方法灵敏度高、重现性好,可用于饮用水中微囊藻毒素的检测。  相似文献   

17.
A rapid and simple method using accelerated solvent extraction and solid-phase extraction cleanup was developed and validated for the determination of 15 organophosphorus pesticides in ginkgo leaves by capillary gas chromatography with flame photometric detection. The pesticides were extracted at 100 degrees C under 1500 psi pressure in <20 min. The average recovery from 10 g ginkgo leaves, fortified at 3 levels ranging from 0.05 to 1.00 mg/kg, was 95.2% with a relative standard deviation of 4.6%. The limits of detection ranged from 1.11 x 10(-3) mg/kg (dimethoate) to 4.44 x 10(-3) mg/kg (dichlorvos). The proposed method showed acceptable accuracy and precision while minimizing environmental concerns, time, and labor. Furthermore, the method could be easily applied to the monitoring of these 15 organophosphorus pesticides in ginkgo leaves.  相似文献   

18.
A PDMS/poly(vinylalcohol) (PDMS/PVA) film prepared through a sol–gel process was coated on stir bars for sorptive extraction, followed by liquid desorption and large volume injection–GC–flame photometric detector (LVI–GC–FPD) for the determination of five organophosphorus pesticides (OPPs) (phorate, fenitrothion, malathion, parathion, and quinalphos) in honey. The preparation reproducibility of PDMS/PVA‐coated stir bar ranged from 4.3 to 13.4% (n = 4) in one batch, and from 6.0 to 12.6% (n = 4) in batch to batch. And one prepared stir bar can be used for more than 50 times without apparent coating loss. The significant parameters affecting stir bar sorptive extraction (SBSE) were investigated and optimized. The LODs for five OPPs ranged from 0.013 (parathion) to 0.081 μg/L (phorate) with the RSDs ranging from 5.3 to 14.2% (c = 1 μg/L, n = 6). The proposed method was successfully applied to the analysis of five OPPs in honey.  相似文献   

19.
固相微萃取/气相色谱-质谱检测纺织品中有机磷农药残留   总被引:3,自引:0,他引:3  
采用PDMS萃取纤维一次吸附富集纺织品中马拉硫磷、甲基对硫磷、敌敌畏、三唑磷、对硫磷、喹硫磷、二嗪磷7种有机磷农药,在气相色谱-质谱(GC-MS)进样口热解吸后进行定性定量检测。筛选了几种商品化的萃取纤维,并优化了萃取时间、萃取温度、吸附时间、盐浓度以及pH值等萃取条件。本方法操作简单、快速、环保,检出限低,可适用于生态纺织品中物质的快速检测。  相似文献   

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