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1.
常常从复杂的多组分混合物的生物和环境样品中分离氯代农药和多氯联苯(PCBs)。分析这些残留物的大多数定性或定量方法包括使用带电子捕获检测器的气相色谱法(ECD-GC)。虽然已报道过许多提取和纯化的方法,但能够成功地自 PCBs 中分离有机氯农药的柱层析纯化技术还没有提出。在含有氯代农药残留和 PCB_5的样品提取物中可以检测出许多峰,但仅仅根据它们的 GC 保留时间不能确切鉴定这些峰是什么。在未经纯化的粗样品提取物中,存在有各种各样的非农药和非多氯联苯残留物,会进一步引起 ECD 的非特征性响应。 相似文献
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《土壤通报》2015,(6):1415-1419
研究建立了土壤中甲氰菊酯、三氟氯氰菊酯、顺式氯菊酯、反式氯菊酯、氯氰菊酯、氟氰戊菊酯、氰戊菊酯和溴氰菊酯8种拟除虫菊酯类农药残留的超声提取-硅胶柱净化-气相色谱(GC)检测方法。以石油醚/丙酮(v/v,2:1)溶液为有机提取剂,超声提取土壤样品,旋转蒸发仪浓缩,经自制硅胶柱以10 ml石油醚/乙酸乙酯(v/v,9:1)溶液进行分离净化并浓缩后用正己烷定容,样品采用气相色谱法FID检测器检测。研究结果表明,该方法对土壤样品中8种拟除虫菊酯的加标回收率较高,平均值在84.9%~101.3%之间。通过实验优化了8种拟除虫菊酯类化合物的分离和测定条件。该提取和检测方法具有简便、快捷、成本低、净化效果和重现性好等特点,适合于土壤中痕量拟除虫菊酯类农药残留的测定。 相似文献
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通过优化ASE萃取参数和固相萃取净化条件,建立了土壤中4种四环素类抗生素残留的加速溶剂萃取-液相色谱串联质谱测定方法。选择EDTA-McIlvaine∶甲醇=1∶2(V/V)作为萃取溶剂,应用Oasis-MAX强阴离子交换柱进行样品的富集和净化,乙腈∶0.4%甲酸溶液=22∶78(V/V)条件下进行色谱分离,ESI正离子源和多反应监测模式(MRM)下测定,方法检测限为2.2～3.2μg.kg-1,定量限为22～32μg.kg-1,样品加标回收率在60.1%～103.8%之间,相对标准偏差为2.6%～4.8%。本方法具较高灵敏度和准确度,能满足土壤中μg.kg-1痕量水平4种四环素类抗生素残留测定要求。 相似文献
5.
2007年3月采集上海市农村及郊区36个表层土壤样品,采用气相色谱法对土壤中的多氯联苯（PCBs）残留进行了分析,揭示了土壤中PCBs的残留水平、分布、组成特征及来源。结果表明,试区土壤中共检出62种PCB,总浓度最高2530ng·kg-1,最低71.7ng·kg-1,平均含量534ng·kg-1。较高污染浓度主要是编号为BS2、SJ6、JS4和FX4的土壤样品,但从整体采样区域来看,其污染可能主要来源于城区污染导致的区域大气沉降或是全球大气传输所致。上海农村及郊区土壤PCBs污染物以Tri-CBs和Tetra-CBs为主,主要以工业Aroclor1242来源为主。相关性分析显示,土壤中PCBs与TOC具有显著相关性,尤其是对于挥发性较强的低氯代PCBs,表明TOC是影响上海市土壤中PCBs持留的重要因素之一。聚类分析显示,部分采样点PCBs污染与工业品使用有关,但可能还存在其他来源。 相似文献
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按照实验室测定油泥污染土壤等复杂介质样品中的多环芳烃分析要求,从消除背景干扰、提高测定数据质量出发,对样品前处理和仪器分析的各环节进行了系统的试验研究,建立了该类污染土壤中多环芳烃的气相色谱-质谱(GC-MS)测定方法,并对该方法进行了质量控制研究.结果表明:针对含油污泥污染土壤中的多环芳烃,该方法对16种多环芳烃的相关系数为0.999 3 ～ 0.999 7,各化合物线性关系良好;最低检出限为0.11 ～ 2.54 ng/ml;回收率为70.5％～107.0％;相对标准偏差为0.09％ ～ 3.15％.本方法能够满足油泥污染土壤等复杂介质样品中的多环芳烃分析要求. 相似文献
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采用磁性石墨烯固相萃取结合超高效液相色谱串联质谱技术,建立了有机肥料中8种镇静剂类和15种β-受体激素药物残留的分析检测方法。样品采用0.1%甲酸乙腈提取,通过磁性石墨烯粉固相萃取吸附目标物,除去杂质,然后再解吸目标物。经Agilent ZORBAX Eclipse Plus C18 (3.0 mm×100 mm,1.8 μm)色谱柱分离,串联质谱进行检测,标准曲线内标法定量。结果表明:23种目标物在0.5～10.0 μg/L范围内线性关系良好(R2>0.999)。在有机肥料样品基质中,目标化合物2、5、10 μg/kg 3个加标水平的平均回收率在75.1%～102.4%之间,相对标准偏差为4.3%～14.3%(n=6)。该方法净化效率高、适用范围广,可用于有机肥料中镇静剂类和β-受体激素类药物残留筛查和检测。 相似文献
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四氢噻吩常用作燃气的气味添加剂,用以追踪燃气的泄露。为建立一套便携式顶空-气相色谱质谱联用法(HS-GC/MS)检测土壤中四氢噻吩浓度的方法,采用正交试验对顶空进样条件(平衡温度、平衡时间和进样压力)和气相色谱质谱检测条件进优化。结果表明,顶空进样的最佳条件为平衡温度80 ℃,平衡时间20 min,进样压力100 kPa。便携式气相色谱质谱联用法(GC/MS)的升温程序：初始柱温60 ℃,保持2 min,以10 ℃/min的速率升至90 ℃,保持4 min,然后以20 ℃/min的速率升至200 ℃,保持10 min。在最佳条件下,方法的检出范围0.005 mg/kg～10.000 mg/kg,不同浓度四氢噻吩的加标回收率为82.4%～98.5%,日内和日间精密度相对标准偏差为4.6%～7.5%,建立的方法快速高效、重复性好,可用于土壤中四氢噻吩现场快速检测。 相似文献
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采用气相色谱串联质谱测定了金华城区20份土壤样品中的7种指示性PCBs（PCB28,PCB52,PCB101,PCB118,PCB138,PCB153,PCB180）,并分析了其分布特征和来源。结果显示金华城区PCBs残留总量在0.111～2.688μg.kg-（1干重）之间,相比国内外其他城市污染程度较轻。和我国其他地区相类似,PCBs的构成中主要以低氯代的三氯联苯和四氯联苯为主,即可能的污染源是我国历史上生产和使用较多的1号PCB,但个别点也显示2号PCB或进口PCBs污染的存在。PCBs污染程度为工业园区〉农田〉公园,说明城市中PCBs的污染源仍是工业园区,其他区域的污染可能来自于大气传播。农田土壤在作物采收后直接暴露在空气污染中,可能是导致其PCBs含量高于公园土壤的主要原因。 相似文献
11.
为快速评价大豆种子活力,该文以人工加速老化后的大豆种子为原料,采用电喷雾萃取电离质谱（extractive electrospray ionization-mass spectrometry,EESI-MS）直接检测不同活力大豆种子水提液,获得其正离子模式下指纹图谱,结合主成分分析（principal component analysis,PCA）、聚类分析（cluster analysis,CA）和判别分析（discriminant analysis, DA）,建立鉴别大豆种子活力的方法。结果表明,在正离子模式下,电喷雾萃取电离质谱结合多变量分析方法可以有效鉴别不同活力大豆种子。主成分分析提取了前3个主成分因子,累计贡献率达到94.80%,聚类分析和判别分析的正确率都为100%,对外部验证样本进行判别分析,正确率为95%。电喷雾萃取电离质谱能快速鉴别不同活力大豆种子,为种子活力检测提供了一种快速、准确、高效的新方法。 相似文献
12.
《Communications in Soil Science and Plant Analysis》2012,43(13-14):1753-1773
Abstract Analytical procedures using gas chromatography–ion trap tandem mass spectrometry (GC‐MS/MS) were developed to analyze atrazine (ATR) and its dealkylated metabolites in four forage species (switchgrass, tall fescue, smooth bromegrass, and orchardgrass). Atrazine, deethylatrazine (DEA), and deisopropylatrazine (DIA) were extracted with methanol (CH3OH) followed by liquid–liquid extraction and partitioning into chloroform, with additional cleanup by C18 solid‐phase extraction (SPE). Through the optimization of ionization conditions and ion storage voltages, the background noise of product ion spectra (MS/MS) was reduced dramatically, providing sub‐µg/kg detection limits. Mean recoveries of ATR, DEA, and DIA were 94.3, 105.6, and 113.1%, respectively. The estimated limit of detection (LOD) was 0.6 µg/kg for ATR, 1.3 µg/kg for DEA, and 0.3 µg/kg for DIA. These LODs were one to two orders of magnitude lower than those reported for other GC‐MS, GC‐MS/MS, high pressure liquid chromatography (HPLC)‐UV, or HPLC‐MS/MS procedures designed for food‐safety monitoring purposes. To validate the developed method, a field experiment was carried out utilizing three replications of four forage treatments (orchardgrass, tall fescue, smooth bromegrass, and switchgrass). Forage plants were sampled for analyses 25 days after atrazine application. DEA concentrations in C3 grasses ranged from 47 to 96 µg/kg, about 10‐fold higher than in switchgrass, a C4 species. The ATR and DIA concentrations were similar, ranging from 1.5 to 13.2 µg/kg. The developed method provided sufficient sensitivity to determine the fate of ATR and its chlorinated metabolites via plant uptake from soil or dealkylation within living forage grasses. It also represented significant improvements in sensitivity compared to previous GC methods. 相似文献
13.
Curie-point pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and in-source pyrolysis-field ionization mass spectrometry
(Py-FIMS) were applied for the first time to the structural characterization of organic nitrogen in hydrolyzates and hydrolysis
residues resulting from the classical 6M HCl hydrolysis of mineral soils. Two well-described soils of widely different origin (i.e., a Gleysol Ah and a Podzol Bh)
were investigated. Py-GC/MS was performed using a nitrogen-selective detector to detect and identify N-containing pyrolysis
in the hydrolyzate (e.g., pyrazole and/or imidazole, N,N-dimethylmethanamine, benzenacetonitrile, propane- and propenenitriles) and the hydrolysis residue (e.g., pyrroles, pyridines,
indoles, N-derivatives of benzene, benzothiazol, and long-chain aliphatic nitriles). Moreover, temperature-resolved Py-FIMS
allowed us to record the thermal evolution of the N-containing compounds during pyrolysis. These were characterized by a particularly
high thermostability compared to their thermal release from whole soils. The combination of pyrolysis with mass spectrometric
methods permitted analyses of the identities and thermal stabilities of complex nitrogen compounds in hydrolysis residues
of whole soils, which cannot be done by wet-chemical methods. Pyrolysis-methylation GC/MS with tetramethyl-ammonium hydroxide
(TMAH) as methylating agent enabled the identification of N,N-dimethylbenzenamine and so confirmed the identification of benzeneamine by Py-GC/MS in nonmethylated hydrolysis residues.
The described N-derivatives of benzene and long-chain nitriles are usually not detectable by pyrolysis-mass spectrometry of
plants and microorganisms. These compounds are characteristic of soils, terrestrial humic substances and hydrolysis residues
and seem to be specific, stable transformation products of soil nitrogen.
Received: 15 April 1996 相似文献
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为建立动物尿液中异丙嗪亚砜、异丙嗪、氯丙嗪、安眠酮和地西泮5种镇静剂类药物残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法,本研究以固相萃取为净化手段,采用HPLC-MS/MS检测猪、牛和羊尿液中5种镇静剂类药物的残留量。结果表明,尿液样品经离心,调节pH值,Oasis MCX固相萃取柱净化后,能够有效去除杂质,5种镇静剂在0.6~20.0 μg·L-1范围内呈良好的线性关系,相关系数(R2)均大于0.993;5种镇静剂类药物的检出限和定量限分别为0.1和0.6 μg·L-1,0.6、2.5和9.0 μg·L-1 3个添加水平的回收率介于64.6%~110.2%之间,相对标准偏差(RSD)均小于6.0%。本研究结果为不同动物尿液中镇静剂类兽药残留的精准检测提供了技术支持。 相似文献
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珠江三角洲典型地区表层农田土壤中多氯联苯残留状况 总被引：7，自引：2，他引：5
采集了珠江三角洲典型区域384个表层农田土壤样品,分析了其中常见6种土壤多氯联苯(PCB28、PCB52、PCB101、PCB138、PCB 153与PCB180)的残留状况.研究结果表明:6种多氯联苯总量(Σ6PCBs)的检出率为78.13％,其平均值为0.42 μg/kg. PCB138的检出率与含量高于其他5种PCBs;土壤中6种多氯联苯的残留状况存在很大的差异;PCB101的检出率最低,仅为10.16％,但其平均值(0.11 μg/kg)较高,主要源于某点位PCB101高达32.44 μg/kg,土壤受到了严重污染.线性相关关系分析结果表明:土壤有机质、黏粒含量则与PCB52存在显著正相关关系.总体而言,低氯代的PCBs含量与土壤理化性质具有一定的相关性,高氯代的PCBs呈现典型的点位污染且在点位土壤中其含量显著高于低氯代同系物. 相似文献
16.
Plant breeders are interested in strawberry species as donors of volatile compounds in breeding programmes because of the
diversity and intensity of wild strawberry aroma. Therefore, the topic of this paper is the prospective analysis of four accessions
of four wild strawberry accessions in comparison to a standard cultivar of Fragaria × ananassa Duch. by using human sensory, gas chromatography mass spectrometry (GCMS) and gas chromatography–olfactometry (GCO). The
wild species have higher aroma intensities compared with the cultivated one. The flavour quality differs significantly. Semiquantitative
GC analysis revealed that F. × ananassa cv. ‘Elsanta’ has the lowest content of volatile compounds whereas Fragaria moschata L. ‘Cotta’ has the highest. The aroma impressions, measured by GCO, support the findings of GCMS analyses. The nasal impact
frequency (NIF)-profiles of the wild types are more manifold and of higher intensities than those of the cultivated F. × ananassa cv. ‘Elsanta’ which corresponds with the overall flavour impression when tasting the fresh fruits. 相似文献
17.
Laschi S Mascini M Scortichini G Fránek M Mascini M 《Journal of agricultural and food chemistry》2003,51(7):1816-1822
In this work, a disposable electrochemical immunosensor, based on a competitive assay scheme, was applied to detect polychlorinated biphenyls (PCBs) in food. For this purpose, antibodies against PCBs were directly immobilized onto the carbon surface of a disposable screen-printed electrode. A competition between the PCBs present in the sample and a fixed concentration of an enzyme-labeled PCB was realized and evaluated by electrochemical detection. Alkaline phosphatase was used as the enzyme label, coupled with differential pulse voltammetry (DPV) as the electrochemical technique. The immunosensor was tested on aroclor mixture detection (1242 and 1248) and then on some typologies of food samples to evaluate the possible application for real sample analysis. Samples analyzed were from different matrixes, such as sheep milk, bovine adipose tissue, and bovine muscle. Results obtained were compared with the accredited results according to ISO 17025 methods for PCB detection (HRGC-LRMS) as a confirmatory analysis. Preliminary results show the possibility to use this device as a screening method in food sample analysis. The negligible matrix effect observed may lead to a simplified extraction procedure, and considerable time and consumable savings are the immediate benefits given by the proposed method. 相似文献
18.
为建立富含二十碳五烯酸(EPA)和二十二碳六烯酸(DHA)型结构磷脂的制备方法,本试验以南极磷虾磷脂为原料,以EPA和DHA总结合率为指标,通过响应面法优化富含EPA/DHA型结构磷脂的酶法合成反应参数,并采用气相色谱(GC)和亲水作用色谱-质谱联用(HILIC-MS)技术对其结构进行表征。结果表明,最优酶催化反应条件为:底物质量比(游离脂肪酸:磷脂, m/m)5.15,反应温度55.22℃,水分添加量(以反应底物总质量计)0.92%,酶添加量(以反应底物总质量计)20%,正己烷3 mL,反应时间24 h,所得结构磷脂中EPA/DHA结合率达64.35%;经GC和HILIC-MS综合分析可知,结构磷脂中磷脂酰胆碱(PC)亚类40:10(20:5/20:5)(18.46%),42:11(20:5/22:6)(12.78%)和38:6(18:1/20:5&16:0/22:6) (7.07%)等分子种含量较高;溶血磷脂酰胆碱LPC亚类20:5(20:5/0:0)(34.40%),22:6(22:6/0:0)(25.99%)和O-16:0(O-16:0/0:0)(10.22%)等分子种含量较高;结构磷脂的PC和LPC组分中脂肪酸单链平均长度≥20的分子种相对含量较原料磷脂分别提高了33.12和37.28个百分点;结构磷脂的PC组分中双键数≥5和双键数≥10的分子种相对含量较原料磷脂分别提高了24.89和27.53个百分点,表明该方法有效提高了结构磷脂中EPA和DHA的含量。本研究结果为进一步探索和丰富酶促合成EPA/DHA型结构磷脂的机理和实践提供了一定的数据支持。 相似文献
19.
With the aid of in-source pyrolysis-field ionization mass spectrometry (Py-FIMS) and Curie-point pyrolysis-gas chromatography/mass spectrometry (cPy-GC/MS) in the conventional electron impact mode, characteristic signals of 23 amino acid standards were described. Thermal and mass spectrometric fragmentation pathways of these amino acids differed with each method and complemented each other. Pyrolysis products assigned by Py-FIMS extended the range of signals for N-containing compounds in humic substances and soil organic matter and gave marker signals for free amino acids and their subunits in proteinaceous materials. These characteristic signals were correlated with the amino acid content in N-rich humic fractions consisting of seven fulvic acids and eight humic acids. The selected marker signals reflected 25–84% of the variances of the molar distribution of acidic, neutral, neutral aromatic, and basic amino acids in the humic fractions. In addition, a well described agricultural soil (0.08% amino acid N) was spiked with a standard amino acid mixture (0.08 mg amino acid N 100 mg-1 dry soil) and produced enhancements of the relative abundances of the corresponding amino acid signals. Moreover, for 27 samples of whole agricultural soils of widely different origins, soil types, and vegetations, 15 selected amino acid indicators were correlated significantly with -amino N (r=0.76***) and total N (r=0.65***). 相似文献
20.
J E Roybal R K Munns W J Morris J A Hurlbut W Shimoda 《Journal of the Association of Official Analytical Chemists》1988,71(2):263-271
A sensitive method is described for the determination and confirmation of zeranol and zearalenone, as well as their isomers and metabolites, in edible animal tissue. The analytes are extracted from tissue with methanol, hydrolyzed enzymatically, cleaned up by acid-base partitioning, determined by liquid chromatography (LC) with electrochemical (EC) detection, and confirmed by gas chromatography/mass spectrometry (GC/MS). LC analysis is performed by isocratic elution with a buffered mobile phase using a Nova-Pak reverse-phase C18 column with amperometric EC detection at +0.90 V. Capillary GC/MS analysis of the trimethylsilyl derivatives provides mass spectral confirmations. 相似文献