首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 140 毫秒
1.
染毒粮食中7种化学战剂的气相色谱分析方法   总被引:5,自引:0,他引:5  
冯翠玲  周永新  胡绪英 《分析化学》2000,28(10):1245-1247
为了研究染毒粮食(大米、面粉)中7种化学战剂的检测方法,建立了相应的气相色谱分析方法。该法采用火焰光度检测器检测,BP-10毛细管色谱柱分离,二氯甲烷萃取。模拟染毒大米、面粉中化学战剂测定相对误差为2.0%~12.0%、8.10%~27.3%。相对标准偏差分别为0.9%~6.10%、3.95%~16.8%。方法的最低检出浓度为0.01~2μg/g。所建方法操作简便,灵敏度高。  相似文献   

2.
在苦味酸盐体系中,用苯并15-冠-5的二氯甲烷溶液可富集萃取Eu^3+;若用0.5mol/L的HNO3溶液反萃取,在反萃取相中仍含有苦味酸根和冠醚;而用隔膜电学反萃取法能有效地将Eu^3+与冠醚和苦味酸根分离,其分离效率达84.8%。  相似文献   

3.
环境和生物样品中多来宝残留量的气相色谱分析方法研究   总被引:3,自引:0,他引:3  
龚道新  杨仁斌  郭正元  沈丹 《色谱》1996,14(6):481-483
 湿性样品中的多来宝残留物用丙酮(水样和干样用石油醚)提取,提取液经石油醚再萃取、浓缩后,用被石油醚饱和的乙腈分配,过硅胶氧化铝混合柱净化,室温下与(CH3)3SiI衍生化反应,生成3-苯氧基苄基碘,用GC检测。当添加浓度为0.05,0.10,1.00μg/g时,样品的平均回收率为80.7%~110.0%,方法最小检出量为0.01ng,样品最小检出浓度是:水0.001mg/L,稻米和土壤0.01μg/g,稻草、谷壳、水浮莲和罗非鱼为0.008μg/g。  相似文献   

4.
环境和生物样品中多来宝残留量的气相色谱分析方法研究   总被引:1,自引:0,他引:1  
湿性样品中的多来宝残留物用丙酮(水样和干样用石油醚)提取,提取液经石油醚再萃取、浓缩后,用被石油醚饱和的乙腈分配,过硅胶氧化铝混合柱净化,室温下与(CH3)3SiI衍生化反应,生成3-苯氧基苄基碘,用GC检测。当添加浓度为0.05,0.10,1.00μg/g时,样品的平均回收率为80.7%~110.0%,方法最小检出量为0.01ng,样品最小检出浓度是:水0.001mg/L,稻米和土壤0.01μg/g,稻草、谷壳、水浮莲和罗非鱼为0.008μg/g。  相似文献   

5.
慕卫 《分析化学》1998,26(5):571-573
提出了用高效液相色谱法同时测定土壤中莠去津、氰草津残留量的方法。用甲醇/乙腈提取,石油醚脱脂,中性氧化铝小柱净化,最后用Nova-PakC16柱进行HPLC分析,流动相:甲醇-水(55+45),吸收波长 228 nm,流速0. 7 mL/min.莠去津最低检出限为 0.3 ng,氰草津为0.2 ng。回收率分别为莠去津83.4%~102.3%,氰草津 82.4%~93.5%.  相似文献   

6.
微生物电极法测定啤酒中乙醇含量   总被引:1,自引:1,他引:1  
用自制的乙醇微生物电极建立了一种测定啤酒中乙醇含量的新方法。该法具有良好的精密度和准确度,其测定结果与比重瓶法和气相色谱法相一致,回收率为97.3%-104.9%。该电极线性范围为0.3-12.0mg/L,60天测定600余次,其灵敏度基本稳定。测试的最适酸度范围为pH6.4-7.3,温度为32-34℃,测定一个样品需5-8min。  相似文献   

7.
本文报告了在0.01mol/LCTAB体系中,以F-为掩蔽剂、苯芴酮显色、用分光光度法测定饮料食品中Ge-132含量,最低检测限0.054μg/mL;线性范围0.54~27.14μg/mL;回收率96.3%~101.5%,并确定了Ge-132摩尔吸收系数(ε)3.39×104。用本法测定了康寿茶、矿泉水和博士奶中Ge-132含量,灵敏度高、重现性和准确度好。用盐酸化本体系,研究了二氧化锗(Ge~(4+))的含量测定,其最低检测限0.021μg/mL;线性范围1.0~21.0μg/ml;回收率95.8%~102.8%,Ge-132不干扰。饮料食品中同时存在Ge-132和Ge(4+)时,本体系可分别测定两者含量。  相似文献   

8.
研究了用HPLC 测定兔眼玻璃体和房水中维拉帕米含量的方法。用丙咪嗪为内标, 采用Spherical C18色谱柱分离, 以甲醇- 0 .04 mol/L 醋酸铵- 乙腈- 二乙胺( 体积比1 ∶1 ∶0 .5 ∶0 .02) 为流动相, 检测波长为278nm 。样品用正己烷- 异丁醇提取后进样, 分析速度快。 样品及内标的保留时间分别为4 .63 min 及9 .23 min ; 线性范围为2 .5 ~100 mg/L, 相关系数r 为0 .999 7 。方法的回收率为100 .3 % ( n = 5) ,RSD 为3 .63% , 日内RSD 为0 .5 % ~3 .61 % , 日间RSD 为3 .75 % ~4 .80 % , 最低检测质量浓度为0.25 mg/ L。 应用该法测定了创伤家兔玻璃体和房水中维拉帕米浓度的变化。  相似文献   

9.
气相色谱/质谱法测定大鼠脑中5-羟色胺的含量   总被引:4,自引:1,他引:3  
梁天天  黄亦佳  朱卡琳 《色谱》1998,16(3):271-273
采用气相色谱/质谱法(GC/MS)测定了正常大鼠和服药大鼠脑组织中5-羟色胺(5-HT)的浓度。大鼠脑组织制成匀浆后,先将5-HT酰化,酰化物经乙酸乙酯提取后,再经七氟丁酸酐衍生化,用GC/MS测定。MS采用电子捕获负离子化学电离(ECNICI)模式。方法的线性范围为0.50~50.0μg/L,回归方程为Y=0.1348X-0.07995(r=0.9996);平均回收率为98.2%±3.8%(n=10);检测限为0.5μg/L;相对标准偏差小于10%。  相似文献   

10.
牟峻  李庆才 《分析化学》1997,25(1):69-71
确立了粮谷和油籽中氯苯胺灵残留量的气相色谱测定方法,试样采用甲醇提取,经与正己烷液液分配,再以弗罗里硅土柱净化,毛细管柱气相色谱-氮磷检测器测定。方法简便、准确、检出限0.02μg/g,添加回收率为87.5-92.9%,相对标准偏差为3.5-7.0%。  相似文献   

11.
气相色谱法测定爱迪注射液中的斑蟊素   总被引:3,自引:0,他引:3  
方伊  张明时 《色谱》2000,18(3):270-271
 研究了斑蟊素在几种萃取体系中的分配行为,测定了它的分配系数。选定二氯甲烷为萃取剂,在相比为1∶10时,只需一次萃取便可以使斑蟊素定量富集。选用OV-17填充柱、外标法定量。方法的分离效果令人满意,检测限低,结果的准确性和精密度良好。  相似文献   

12.
Ultrasonic extraction was used to develop a suitable binary solvent system for the analysis of synthetic pyrethroid pesticides and mirex on soil. The analysis was carried out by gas chromatography with negative ion chemical ionization mass spectrometry (GC/MS-NICI). In the initial experiments, accurately weighed soil samples were spiked with a mixture of standard solution pyrethroids and mirex and shaken for 24?h to ensure homogeneity, then extracted with solvent. The extracts were evaporated to dryness before the volumetric internal standard was added.

The binary solvents used in this study were various mixtures of hexane?:?acetone, hexane?:?dichloromethane (DCM), isooctane?:?acetone and isooctane?:?dichloromethane, representing different classes of polarity. The recoveries of all pyrethroids and mirex were satisfactory over three solvent systems: hexane?:?acetone, hexane?:?DCM and isooctane?:?acetone, but results of isooctane?:?DCM produced low recoveries. The average recovery increased with the extraction time, but the increase was not statistically significant. A 30-min optimum extraction was deemed sufficient for recovering pyrethroids from soil. After 30?min, extraction decreased owing to the re-distribution of the analyte on the soil matrix.  相似文献   

13.
建立了一种测定甘蔗和土壤中敌草隆农药残留的超高效液相色谱(UPLC)方法.样品经水和甲醇提取,二氯甲烷液-液分配后,过中性氧化铝柱纯化,用石油醚:乙酸乙酯的混合液(体积比85:15)淋洗和洗脱,洗脱液经减压浓缩后用5 mL乙腈定容.采用UPLC分离,紫外检测器检测,外标法定量.敌草隆在0.02~5.0 mg/L范围线性...  相似文献   

14.
Dost K  Jones DC  Auerbach R  Davidson G 《The Analyst》2000,125(10):1751-1755
This paper presents an analytical technique for the determination of pesticides in soil by packed-column supercritical fluid chromatography interfaced with atmospheric pressure chemical ionisation mass spectrometry (pSFC-APCI-MS). The technique provides a versatile method for the detection and quantification of pesticides belonging to three different commonly used classes, triazines (ametryne, atrazine), carbamates (carbofuran) and sulfonylureas (chlorsulfuron, metsulfuron methyl and benzsulfuron methyl). The APCI mass spectra for all the pesticides studied consisted of protonated molecule ions as the most abundant ion at low cone voltages, except for metsulfuron methyl and benzsulfuron methyl, which gave a fragment ion as the most abundant ion with the protonated molecule ion at low intensity. Increasing the cone voltage provided informative fragmentation patterns for all species. The technique shows good linearity over the concentration range of 0.1-50 micrograms ml-1, with r2 values as follows: atrazine 0.997, ametryne 0.995, carbofuran 0.999, benzsulfuron methyl 0.999, chlorsulfuron 0.995 and metsulfuron methyl 0.997. The detection limits in the selected ion mode were atrazine 201, ametryne 144 and carbofuran 385 pg, which were calculated by using the standard solution, and benzsulfuron methyl 2.045, chlorsulfuron 1.435 and metsulfuron methyl 2.414 ng, which were determined by using spiked soil samples. The pSFC-MS system was shown to have a high degree of reproducibility. The technique was then applied to the determination of the above pesticides in soil samples. The results obtained show that there is no matrix effect from the soil and that the detection limits for all pesticides in soil were similar to those found for the standard solutions.  相似文献   

15.
A relatively simple method for the determination of azoxystrobin residues in grapes and soil using gas chromatography equipped with electron capture detector (GC-ECD) is described. Samples were extracted with acetone, and further partitioned with dichloromethane and petroleum ether. The extracts were then cleaned up in a glass clean-up column filled with active charcoal and silica gel, and eluted with dichloromethane/ethyl acetate (70:30, v/v). The eluate was collected and concentrated for GC-ECD analysis. The results showed good linearity (r 2 = 0.9998) over the concentration range of 6.25–400 ng mL?1. The limits of detection (LOD) and quantification (LOQ) of azoxystrobin were 3 and 10 ng mL?1. Recovery from soil and grape samples was in the range of 83.52–107.36 and 82.21–107.31%, with corresponding relative standard deviations (RSD) of 5.21–9.11 and 4.53–5.90% for the three fortified levels. Inter- and intra-day RSDs were in the range of 0.87–6.76 and 2.01–5.46%. The accuracy and sensitivity of the GC-ECD method was independently confirmed by LC and GC-MS. It was demonstrated that the proposed method was simple and efficient, and particularly suitable for detecting azoxystrobin residues in grapes and soil.  相似文献   

16.
Nine volatile halogenated organic compounds (VHOCs), including four trihalomethanes (THMs), were determined in soils by capillary gas chromatography with microwave induced-plasma atomic emission spectrometry (GC-AED), using a purge-and-trap system (PT) for sample preconcentration. Analytes were previously extracted from the soil sample in methanol and the extract was preconcentrated before being chromatographed. Element-specific detection and quantification were carried out monitoring two wavelength emission lines, corresponding to chlorine (479 nm) and bromine (478 nm). Each chromatographic run took 21 min, including the purge step. The method showed a precision of 1.1-7.2% (R.S.D.) depending on the compound. Detection limits ranged from 0.05 to 0.55 ng ml−1, for chloroform and dichloromethane, respectively, corresponding to 3.3 and 36.0 ng g−1 in the soil samples. The chromatographic profiles obtained showed no interference from co-extracted compounds. Low levels of dichloromethane and chloroform ranging from 0.04 to 1.13 μg g−1 were found in samples obtained from small gardens irrigated with tap water. The method is reliable and can be used for routine monitoring in soil samples.  相似文献   

17.
土壤中痕量酞酸酯的提取与分析方法研究   总被引:5,自引:0,他引:5  
采用CH_2Cl_2超声提取、氧化铝、硅胶双柱净化、高效液相色谱(HPLC)测定土壤中的酞酸酯(PEs)、标准添加回收率达93%~106%,对超声提取与索氏提取进行了比较,并对实际土壤样品中的PEs进行了初步分析。  相似文献   

18.
Summary A method is described for the determination of polycyclic aromatic hydrocarbons in natural soil. The soil is dried and extracted by ultrasonic agitation with dichloromethane. The extract is purified by liquid-liquid partitioning with dimethylformamide, water and hexane followed by high performance liquid chromatography on a silica column. Quantitative analysis of the purified extract is carried out by combined gas chromatography/mass spectrometry. The method yields reliable results at the ng/g level.
Bestimmung von Spuren polycyclischer aromatischer Kohlenwasserstoffe in Boden
  相似文献   

19.
采用气相色谱/质谱法直接测定了卷烟主流烟气中的1-氨基萘、 2-氨基萘、 3-氨基联苯和4-氨基联苯等4种芳香胺.该方法直接用CH2Cl2溶剂超声振荡萃取滤片中的芳香胺,超声萃取的同时加入衍生试剂,使萃取和衍生化同步进行,萃取液过硅酸镁柱进行进一步纯化,然后旋转浓缩后进行GC/MS分析.方法的RSD在1.0%~3.7%之间,加标回收率在92.9%~101.1%之间.  相似文献   

20.
Summary Gas chromatographic conditions for determining eight phenylurea (chlortoluron, diuron, fluometuron, isoproturon, linuron, metabenzthiazuron, metobromuron and monuron) and one sulfonylurea (chlorsulfuron) herbicides were assessed. Degradation products of the herbicides formed in the injector were used for identification. Most phenylureas formed their respective carbamic acid methyl esters, metabenzthiazuron formed an aminobenzothiazol and chlorsulfuron formed an aminotriazine plus a phenylsulfonamide. On-column injection of standards using a BP10 capillary column was evaluated to identify the chromatographic behaviour. Detection limits ranged from 0.05 ng for chlorsulfuron to 3 ng for monuron with the NPD and, from 0.01 ng for chlorsulfuron to 5 ng for metabenzthiazuron with the ECD. The RSDs (n=4) were lower than 4% at the 12–25 ng level. The method was applied to the analysis of surface waters extracted with C18 Empore disks with recoveries higher than 85%. Each herbicide could be determined in water down to 0.1 μg·L−1. Chlortoluron was found (11.4 μg·L−1) in a water sample and its presence was confimed by gas chromatography-mass spectrometry.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号