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1.
林蛙油中农药残留的GC-MS/MS检测方法 总被引:3,自引:0,他引:3
首次建立了林蛙油中15种农药(p,p′DDE,O,p′-DDD,o p′-DDT,p,p′-DDT,BHC(α、β、γ、δ),异丙威,甲拌磷,六氯苯,百菌清,皮蝇磷,倍硫磷,甲氰菊酯)的GC—MS/MS残留检测方法。样品用乙酸乙酯提取、Florisil层析柱净化后,经GC—MS/MS检测,用外标法定量。15种农药在0.050~10.0mg/L范围内,线性关系良好,相关系数r≥0.996。当添加量在0.050—2.00mg/kg间,平均加标回收率为81%~117%,RSD为2.4%-18.2%,方法的检出限为0.050mg/kg。该方法准确、灵敏,适用于农药残留的分析。 相似文献
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基质固相分散和GC-NCI-MS法分析果汁中拟除虫菊酯农药残留量 总被引:2,自引:0,他引:2
建立了基质固相分散法(MSPD)和气相色谱-负化学离子源-质谱法(GC—NCI—MS)应用于果汁中10种拟除虫菊酯农药残留量的快速分析方法,并对这些农药NCI—MS的阴离子结构与断裂机理进行初步探讨。采用以中性氧化铝为吸附刺、Florisil硅藻土为净化剂和乙酸乙酯为洗脱剂的MSPD样品前处理方法,以PCB103为内标物和GC—NCI—MS的选择离子监测方式(SIM)进行定性与定量分析。当样品的加标浓度水平为50、250μg/kg时,平均加标回收率为86.7%~114.8%,相对标准偏差为1.9%~14.1%;除氯菊酯农药的方法检出限(MDL)为14.7μg/kg外,其余农药的MDL大都小于1.0μg/kg;线性范围为10~500μg/kg,相关系数都大于0.997,在所分析的大部分果汁中至少分析出两种以上的拟除虫菊酯农药残留。 相似文献
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凝胶渗透色谱-气相色谱-质谱测定玉米中3种农药的残留 总被引:14,自引:1,他引:14
建立以凝胶渗透色谱(GPC)和气相色谱-质谱(GC/MS)联用技术测定玉米中三唑酮、三唑醇-a,三唑醇-b残留量的方法。目标农药经乙腈提取,共提物中的油脂经液/液分配、GPC加以去除,叶黄素通过固相萃取(SPE)净化。目标农药采用GC/MS/SIM方式进行定性、定量分析。3种农药(0.05、0.5、2μs/s)的回收率在90%-110%;相对标准偏差(RSD)〈10%。 相似文献
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气相色谱质谱联用法对农产品中8种种衣剂农药残留的同时测定 总被引:2,自引:0,他引:2
应用气相色谱-质谱联用仪(GC-MS)建立了水果、蔬菜、粮谷等农产品中8种种衣剂农药残留的分析测定方法。样品用乙腈提取,通过石墨化碳或C18固相萃取小柱净化,经DB-5ms气相色谱柱分离,电子轰击电离(EI)、选择离子监测模式(SIM)对定量离子和定性离子进行MS测定。标准工作曲线范围0.02-0.5mg/L。样品中添加水平为0.005、0.010和0.020mg/kg时,回收率为74%~110%;相对标准偏差小于15%。检出限(S/N=3)为0.09~0.77μg/kg。 相似文献
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凝胶渗透色谱-气相色谱质谱法测定:花生中6种除草剂农药残留 总被引:1,自引:0,他引:1
建立了凝胶渗透色谱一气相色谱质谱(GPC~GC=MS)法测定花生中6种除草剂(氟乐灵、异恶草酮、甲草胺、二甲戊乐灵、乙氧氟草醚、喹禾灵)农药残留的方法。样品经乙腈提取,氨基固相萃取柱和凝胶渗透色谱净化,在选择离子扫描(SIM)模式下进行气相色谱质谱法测定,外标法定量。6种除草剂浓度在0.02-1.00mg/L范围内与色谱峰面积呈良好的线性,线性相关系数为O.9949~0.9998,添加回收率为77.8%-101.6%,测定结果的相对标准偏差为4.4%~11.4%(月=5),方法的检出限为0.1~1.3μg/kg。 相似文献
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固相微萃取/气相色谱/质谱联用技术在农药残留物分析中的应用 总被引:25,自引:2,他引:23
综述了固相微萃取/气相色谱/质谱(SPME/GC/MS)在各种环境水、土壤等样品中农药残留分析中的应用和发展。SPME/GC/MS联用技术具有快速、简便、准确等优点。 相似文献
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超高效液相色谱串联质谱法测定银杏中氨基甲酸酯类农药残留 总被引:1,自引:0,他引:1
建立了银杏叶中15种氨基甲酸酯类农药残留量的超高效液相色谱一串联质谱测定方法。样品经乙腈提取,TPT固相萃取柱净化,通过XTerra MS Cl8色谱柱分离,供串联质谱测定。15种氨基甲酸酯类农药在0.02-0.5mg/L范围内线性良好,相关系数为0.9962-0.9999;在0.004,0.01,0.02,0.04mg/kg4个添加水平下,其平均回收率为65.22%-96.66%,相对标准偏差为1.43%-10.06%(n=5)。该方法净化效果好、灵敏度高、重现性好,可满足银杏叶中15种氨基甲酸酯类农药残留量的检验要求。 相似文献
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大豆中二硝基苯胺类除草剂多残留的气相色谱法定量检测及质谱确证 总被引:3,自引:0,他引:3
建立以凝胶渗透色谱法(GPC)和固相萃取法(SPE)及气相色谱法(GC)联用技术测定大豆中10种二硝基苯胺类除草剂(氟乐灵、乙氟灵、环丙氟、氯乙氟灵、仲丁灵、异乐灵、二甲戊乐灵、二硝胺、氨基丙氟灵和磺乐灵)多残留检测方法。目标农药经正己烷饱和的乙腈提取,凝胶渗透色谱除去大豆中大部分油脂及色素,再经Florisil柱净化和富集,依次用6mL二氯甲烷和6mL二氯甲烷+丙酮(99+1)洗脱。目标农药采用电子捕获检测(GC/ECD),外标法定量,并经质谱(MS)确证。两个添加水平重复6次,回收率分别为74%~105%和59%~105%;相对标准偏差〈20%;检出限为1.8~7.6μg/kg;定量限为6~38μg/kg。 相似文献
11.
利用手持技术改进测定乙醇分子结构实验 总被引:1,自引:0,他引:1
利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。 相似文献
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由于石化行业的生产需要,其材质的使用具有多样性和广泛性,经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识,根据光谱仪的测试能力及标样的采集,实现了一个或几个元素测量范围的扩展,并对其测量的影响因素进行了研究。 相似文献
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V. I. Bol'shakova L. I. Demenkova É. N. Shmidt V. A. Pentegova 《Chemistry of Natural Compounds》1989,24(6):691-694
The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988. 相似文献
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Mustafa R. Ibrahim Zacharia A. Fataftah Paul von Ragu Schleyer Peter D. Stout 《Journal of computational chemistry》1987,8(8):1131-1138
Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases. 相似文献
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V. I. Bol'shakova L. I. Demenkova É. N. Shmidt V. A. Pentegova 《Chemistry of Natural Compounds》1988,24(6):691-694
The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae. 相似文献
19.
Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin
E. I. Kapinus V. A. Ganzha B. M. Dzhagarov E. I. Sagun V. B. Pavlenko 《Theoretical and Experimental Chemistry》1989,25(2):146-151
The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989. 相似文献
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The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted
indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator
model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was
established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing
analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997. 相似文献