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51.
52.
超高效液相色谱-质谱/质谱法测定叶菜中11种氨基甲酸酯农药残留 总被引:2,自引:0,他引:2
建立了采用固相萃取-超高效液相色谱-质谱/质谱法(SPE-LC-MS/MS)对叶菜中11种氨基甲酸酯农药(克百威、3羟基克百威、甲萘威、仲丁威、异丙威、抗牙威、速灭威、灭多威、涕灭威、涕灭威亚砜、涕灭威砜)残留同时测定的方法。样品用乙腈提取后经氨基固相萃取柱净化处理,经Acquity UPLCTM BEH C18(100 mm×2.1 mm,1.7μm)色谱柱分离后测定,该方法采用多反应监测(MRM)离子扫描模式,外标法进行定量,线性良好(r2>0.994),检出限为0.001~0.004 mg/kg,总体回收率为80.4%~99.8%,相对标准偏差为3.4%~10.8%。该方法的定量限满足目前国内外药物的最大残留限量要求,可作为叶菜中相关药物残留的筛选检测方法。 相似文献
53.
[目的]建立一种测定红酒中氨基甲酸甲酯(MC)的高效液相色谱-质谱联用法(HPLC-MS)。[方法]对样品采用0.45μm微孔滤膜过滤后,用氨基固相萃取小柱进行提取、纯化和氮吹浓缩处理,然后用HPLC-MS进行定性定量分析。HPLC条件为:色谱柱,氰基农残色谱柱(250 mm×4.60 mm i.d.,5μm);流动相,乙腈-水(0.1%乙酸)80∶20;流速0.8 ml/min;检测波长195 nm;柱温25℃;进样量20μl。质谱条件:离子源为电喷雾离子源(ESI+源),扫描方式为正离子扫描,干燥气流速为8.0 L/min,干燥气温度为350℃,扫描范围为50~200 m/z,雾化气压力为275.8 kPa。[结果]MC在0.1~20μg/ml范围内线性关系良好,相关系数r为0.996 0。平均回收率为83.40%,RSD为6.8%。[结论]所建立的方法具有较好的精密度和准确度,并具有样品处理简单、检测限低、分析时间短等特点,适于红酒中MC的测定。 相似文献
54.
为了寻找新的含噻唑杂环的先导化合物,利用2-硫代-1,3-噻唑烷与氯甲酸酯在三乙胺存在下进行缩合反应,合成了11个2-硫代-1,3-噻唑烷-3-甲酸酯类化合物,并利用1H NMR、IR、 MS及元素分析对其结构进行了表征;通过X-ray单晶衍射测定了2-硫代-1,3-噻唑烷-3-甲酸苯酯( 3i )的晶体结构,证实反应产物为硫酮式而非硫酯式结构。 初步生物活性试验结果表明,在试验浓度下部分目标化合物具有一定的杀菌和杀虫活性,其中 3c、3f、3h、3k 在500 mg/L下对棉红蜘蛛Tetranychus urticae的致死率均在70%以上。 相似文献
55.
Esther Fernández Carolina Grávalos Pedro Javier Haro Dina Cifuentes Pablo Bielza 《Pest management science》2009,65(8):885-891
BACKGROUND: Bemisia tabaci Gennadius Q‐biotype has readily developed resistance to numerous insecticide classes. Studies in the Mediterranean area are needed to clarify the resistance status and cross‐resistance patterns in this invasive whitefly biotype. The levels of resistance in nymphs of seven strains of B. tabaci Q‐biotype from south‐eastern Spain to representative insecticides were determined. RESULTS: Six populations had low to moderate levels of resistance to azadirachtin (0.2‐ to 7‐fold), buprofezin (11‐ to 59‐fold), imidacloprid (1‐ to 15‐fold), methomyl (3‐ to 55‐fold), pyridaben (0.9‐ to 9‐fold), pyriproxyfen (0.7‐ to 15‐fold) and spiromesifen (1‐ to 7‐fold), when compared with a contemporary Spanish Q‐biotype reference population (LC50 = 2.7, 8.7, 15.2, 19.9, 0.34, 20.9 and 1.1 mg L?1 respectively). A single population collected from a greenhouse subject to intensive insecticide use exhibited generally higher resistance levels to the same array of compounds (31‐, 1164‐, 3‐, 52‐, 9‐, 19‐ and 3‐fold respectively). Pyridaben and spiromesifen were extremely effective against nymphs of all strains, with LC50 values significantly below recommended application rates. CONCLUSION: In contrast to previous reports, high rates of efficacy exist for numerous insecticide classes against B. tabaci Q‐biotype populations in these intensive agricultural regions of south‐eastern Spain. This probably reflects the recent and significant reductions in exposure that have resulted from a wider uptake of IPM technologies and strategies. However, the continued presence of resistance genes also suggests that a reversion to levels of high insecticide exposure could result in a rapid selection for resistance. Copyright © 2009 Society of Chemical Industry 相似文献
56.
Samples of housefly (Musca domestica) field populations were collected from Danish livestock farms in 1997. The tolerance of the first‐generation offspring was determined for a number of insecticides. Dose‐response values were obtained by topical application for the pyrethroids bioresmethrin and pyrethrum, both synergised with piperonyl butoxide, and the organophosphate dimethoate. The organophosphates azamethiphos and propetamphos and the carbamate methomyl were tested in discriminating dose feeding bioassays. Resistance was low to moderate in most of the populations for most of the compounds tested, but this study also revealed the existence of high resistance to pyrethroid, organophosphate and carbamate insecticides in some populations. The resistance factors at LD50 for bioresmethrin/piperonyl butoxide ranged between 2 and 98, and for pyrethrum/piperonyl butoxide between 2 and 29. Our results indicate that pyrethroid resistance in Denmark is increasing, since four of the 21 farms showed more than 100‐fold resistance at LD95, a level of resistance only observed once before. Resistance factors at LD50 for dimethoate ranged from 9 to 100, and showed two distinct trends: populations with either decreasing or increasing resistance. Resistance to azamethiphos was found to be widespread and high. Although two strains with high methomyl and propetamphos resistance were observed, methomyl and propetamphos resistance is moderate and appears not to be increasing. © 2001 Society of Chemical Industry 相似文献
57.
为简化液相色谱法测定氨基甲酸酯类农药残留的前处理步骤,提高检测效率,采用Q u E C h E R S提取高效液相色谱法建立了菜薹中10种氨基甲酸酯类农药的快速检测方法。样品经乙腈提取后,经提取液氮吹浓缩、多功能针式过滤器净化并进样分析,采用加标回收的方法测定回收率和精密度,检验其准确性和可靠性。结果显示:10种氨基甲酸酯农药回收率为70.9%~101.5%,相对标准偏差(RSDs)为1.7%~6.2%,证明检测方法简单、快速,可满足菜薹中10种氨基甲酸酯类农药残留的检测工作。 相似文献
58.
建立QuEChERS-气相色谱-串联质谱法测定豆乳中12 种有机磷及氨基甲酸酯类农药残留的方法。样品经乙腈提取,柠檬酸盐缓冲条件下分离,无水硫酸镁、乙二胺-N-丙基硅烷化硅胶和C18净化处理,气相色谱-串联质谱仪测定。结果表明:12 种农药的定量限均为0.004 mg/kg;标准曲线在5~200 ng/mL范围内线性良好,相关系数>0.99;进行3 个不同水平的加标实验,加标回收率为71.8%~114.9%,相对标准偏差为4.6%~13.3%。该方法快速、高效、准确,可用于豆乳中有机磷及氨基甲酸酯类农药残留的测定。 相似文献
59.
Seven field populations of mosquito Culex pipiens complex (Diptera: Culicidae) were collected from four provinces of China. The resistance status of larvae to dichlorvos, parathion, chlorpyrifos, fenobucarb (BPMC) and propoxur were determined by bioassays, disclosing that they were more resistant to organophosphate (moderate or low resistance) than to carbamate (low or no significant resistance) insecticides. Starch gel electrophoresis confirmed the presence and distribution of overproduced esterases B1, A2-B2, A8-B8 and A9-B9, the frequencies of which varied according to their regional origins. Electrophoretic polymorphism at four putatively neutral loci (got-1, got-2, pgi and pgm) showed that the overall genetic differentiation found across all populations was significantly large (Fst = 0.28, P < 10(-4)), and genetic exchange was slightly restricted by distance isolation (P = 0.018). 相似文献
60.
BACKGROUND: Pyrethroid insecticides have historically been effective for controlling bean leaf beetles in soybeans. Perceived field efficacy in the Mississippi Delta region has been lower over the past several years. Laboratory and field data were collected to determine whether there has been a reduction in pyrethroid insecticide susceptibility. RESULTS: Laboratory and field data both confirmed that control of bean leaf beetles with pyrethroid insecticides is poorer in the Delta regions of Mississippi and Louisiana than in all other regions tested. However, it was not possible to show that this reduced susceptibility changed over time. Furthermore, insect movement appeared to make insecticide susceptibility regional, so that localized insecticide applications had little impact on the susceptibility of successive generations. CONCLUSION: Lack of field control owing to low efficacy of pyrethroid insecticides against bean leaf beetle populations in the Delta region should be expected. Selection pressure on a regional basis may further decrease efficacy. Carbamate insecticides generally still provide high levels of control. Copyright © 2011 Society of Chemical Industry 相似文献