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1.
气相色谱-氮磷检测器测定草甘膦在土壤和苹果中的残留量 总被引：6，自引：1，他引：5
建立了简单、灵敏的土壤及苹果中草甘膦残留量的气相色谱检测方法。土壤样品用2 mol/L 的氨水提取,经三氟乙酸酐(TFAA)和三氟乙醇(TFE)衍生化后,由配有氮磷检测器的气 相色谱(GC-NPD)进行检测。土壤中草甘膦的最小检出量为9×10-12 g,最低检出浓度为0.02 mg/kg, 平均回收率及变异系数分别为84.4% ~94.0% 和7.46% ~10.40%。苹果样品则采用去离子水提取,经二氯甲烷液液分配和BIO-RAD AG 50W-X8阳离子交换柱净化后,再用TEAA和TFE衍生化,最后用GC-NPD检测,其中草甘膦的最小检出量(LOD)和最低检出浓度(LOQ)与土壤样品中的相同,平均回收率及变异系数分别为80.7% ~98.6%和9.3% ~11.8%。草甘膦的衍生化产物通过气相色谱-质谱联用仪(GC-MS)进行了确证。在北京昌平地区进行的消解动态和最终残留试验结果表明,以推荐高剂量(有效浓度)的1.5倍(2 025 g/hm2)施药,草甘膦在土壤中的半衰期为 9.2 d。两年的最终残留试验结果表明,无论是高浓度区(2 025 g/hm2)还是低浓度区(1 350 g/hm2),苹果收获时(距施药75 d),土壤和苹果样品中均未检出草甘膦。 相似文献
2.
Mahdi Najafi-Ghiri Abbas Mirsoleimani Hossein Amin 《Arid Land Research and Management》2017,31(4):431-445
Nutrient deficiency may be a reason for citrus decline in many countries. In the current investigation, soil and leaf samples of 63 Washington Navel orange orchards in arid lands of southern Iran (Darab region) were analyzed to study the nutritional status of orange orchards and to find relationships between soil properties and nutrients content of soils and orange leaves. The soils differed widely in clay content (3–37%), pH value (7.04–7.95), calcium carbonate equivalent (18–86%), and organic matter content (0.3–12%). These soils represented a wide range of plant nutrients concentration. Majority of the studied soils had sufficient concentrations of all nutrients (except Fe). Results indicated that pH, organic matter, clay, and calcium carbonate contents are the most important characteristics that control the soil nutrients availability. The mean contents of N, K, P, Fe, Mn, Zn, and Cu in leaves were 2.59, 0.84, and 0.14% and 66, 44, 17, and 12?mg?kg?1, respectively. Most orchards showed K, Fe, and Zn deficiencies. We found no relationships between nutrients content in leaf and soil (except for K, Mn, and Zn); and this indicated that soil analysis may not be a reliable method for most nutrient deficiency diagnosis. 相似文献
3.
单嘧磺隆在土壤中的残留分析和消解动态研究 总被引：12，自引：1，他引：11
研究了新磺酰脲除草剂单嘧磺隆在土壤中的残留分析方法及其土壤消解动态和最终残留。土壤经甲醇和稀氨水混合液提取 ,液液分配及 C18净化 ,浓缩后用带紫外检测器的高效液相色谱仪进行测定。单嘧磺隆的最低检出量为 4 ng,在土壤中的最低检出浓度为0 .0 2 mg/ kg。本方法的添加回收率为 95.10 %～ 10 3.77% ,变异系数为 1.4 7%～ 11.80 % ,符合农药残留分析的要求。运用上述方法 ,测定了单嘧磺隆在北京和山东土壤中的消解动态以及最终残留。结果表明 :单嘧磺隆在土壤中消解的速度较慢 ,在北京土壤中的半衰期为 9.2 4 d,山东土壤中的半衰期为 13.59d。按推荐剂量施药 ,小麦收获时 ,在北京和山东两地土壤中均未检出单嘧磺隆。 相似文献
4.
本研究首次建立了一种超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定柑橘中草甘膦及其代谢物N-乙酰草甘膦?氨甲基磷酸(AMPA)和N-乙酰AMPA?样品经过0.5%甲酸水提取, 以十八烷基硅烷键合硅胶柱(C18)净化, 利用水和200 mmol/L碳酸氢铵溶液(含0.1%氨水)作为流动相梯度洗脱, 在多反应监测模式下定量分析?结果表明, 草甘膦及其代谢物在0.05~1 mg/kg范围内线性关系良好, 相关系数均大于0.99; 草甘膦及其3个代谢物在柑橘全果和果肉基质中3个加标水平下回收率为 70.5%~109.5%, 相对标准偏差(RSD)为0.6%~10.1%, 定量限为0.05 mg/kg?本方法的前处理样品无需衍生, 简便?快捷?高效?准确可靠, 可用于柑橘中草甘膦及其代谢物N-乙酰草甘膦?AMPA和N-乙酰AMPA的定量检测? 相似文献
5.
Philip Eberbach 《Pest management science》1998,52(3):229-240
The decomposition behaviour of glyphosate in four Victorian soils was investigated at two temperatures using non-steady-state compartmental analysis. At 25°C, glyphosate degradation was shown numerically to be derived from two different sources where the rate of release from each source behaved in accordance with first-order kinetics. Over the first 40 day period for each of the soils, glyphosate was derived simultaneously from the labile and non-labile phase, whilst after the first 40 days, glyphosate was derived solely from the non-labile phase. At this temperature, the amount of glyphosate partitioned into the labile phase ranged from 24·1 to 34·5%, whilst the amount partitioned into the sorbed, non-labile phase ranged from 67·2 to 74·9%. The half-lives for glyphosate within each phase was calculated and ranged from six to nine days for the labile phase to 222–835 days for the non-labile phase. Glyphosate appeared to be more strongly held in the acidic Rutherglen soil than in the alkaline soils studied, and this was thought to be related to the substantially lower pH and higher Fe content of the acidic soil. At 10°C, glyphosate was shown numerically to be derived from two different sources for two of the soils. However, for the two remaining soils, glyphosate appeared to be derived either from a single phase or from two phases at either the same rate or at differential rates where the rate of release from one phase was sufficiently fast to mask the rate of release from the other. At this temperature, more glyphosate was partitioned into the non-labile phase of the Walpeup and Rutherglen soils than at 25°C. However, the rate of release of glyphosate from this phase increased for the Walpeup soil relative to that at 25°C, but decreased substantially for the Rutherglen soil. This suggests that different mechanisms for the binding of glyphosate into the non-labile phase may exist between soils. © 1998 SCI. 相似文献
6.
Although glyphosate (N‐(phosphonomethyl)glycine) is one of the most frequently used herbicides, few controlled transport experiments in undisturbed soils have been carried out to date. The aim of this work was to study the influence of the sorption coefficient, soil‐glyphosate contact time, pH, phosphorus concentration and colloid‐facilitated transport on the transport of [14C]glyphosate in undisturbed top‐soil columns (20 cm height × 20 cm diameter) of a sandy loam soil and a sandy soil. Batch sorption experiments showed strong Freundlich‐type sorption to both soil materials. The mobility of glyphosate in the soil columns was strongly governed by macropore flow. Consequently, amounts of glyphosate leached from the macroporous sandy loam soil were 50–150 times larger than from the sandy soil. Leaching rates from the sandy soil were not affected by soil‐glyphosate contact time, whereas a contact time of 96 h strongly reduced the leaching rates from the sandy loam soil. The role of pH and phosphorus concentration in solution was relatively unimportant with respect to total glyphosate leaching. The contribution of colloid‐facilitated transport was <1 to 27% for the sandy loam and <1 to 52% for the sandy soil, depending on soil treatment. The risk for glyphosate leaching from the top‐soils seems to be limited to conditions where pronounced macropore flow occurs shortly after application. © 2000 Society of Chemical Industry 相似文献
7.
建立了以4-氯-7-硝基苯并呋喃 (NBD-Cl) 柱前衍生为基础测定土壤中草甘膦残留的高效液相色谱法。土壤样品经0.6 mol/L KOH溶液提取，加入NBD-Cl衍生剂，在0.125 mol/L (pH = 9.0~10.5) 硼酸盐缓冲液介质中、60 ℃水浴条件下反应80 min。以0.02 mol/L V (磷酸氢二钠水溶液) : V (甲醇) = 70 : 30的混合溶液为流动相，经C18反相色谱柱分离后，采用二极管阵列检测器在500 nm波长处进行检测，外标法定量。结果表明:草甘膦在0.01~2.0 mg/L 范围内线性关系良好，相关系数为0.9999，定量限 (LOQ) 为0.02 mg/kg；向空白土壤样品中添加0.02、0.1和10 mg/kg 3个水平的草甘膦标准溶液，平均回收率在82%~93%之间，相对标准偏差 (RSD) 为2.5%~3.9%。该方法简便高效，适用于土壤样品中草甘膦的残留分析。 相似文献
8.
Adsorption-desorption of the herbicide flufenacet (FOE 5043) has been studied in five soils from different locations in India (Delhi, Ranchi, Nagpur, Kerala and Assam) varying in their physicochemical properties. The organic matter (OM) content varied from 0.072 to 0.864%, clay content from 2.5 to 43.7% and pH from 4.45 to 8.35. The adsorption studies were carried out using a batch equilibration technique. Ten grams of soil were equilibrated with 20 ml of aqueous 0.01 M CaCl2 solution containing different concentrations (0-30 mg litre-1) of flufenacet. After equilibration, an aliquot of supernatant was taken out for analysis. During desorption, the amount withdrawn for analysis was replenished with fresh 0.01 M CaCl2 solution and further equilibrated. Desorption studies were carried out with the 30 mg litre-1 concentration of flufenacet only. The adsorption studies revealed that there was moderate to high adsorption of flufenacet considering the comparatively low organic carbon content in the five test soils. Average Kd values ranged from 0.77 to 4.52 and Freundlich KF values from 0.76 to 4.39. The highest adsorption was observed in Kerala soil (OM 0.786%; clay 25%; pH 4.45) followed by Ranchi, Nagpur and Delhi soils, and the lowest in Assam soil (OM 0.553%; clay 2.5%; pH 6.87). The trend in adsorption could be attributed to the chemical nature of flufenacet and the physicochemical properties of the soil such as pH, OM and clay contents. OM and clay contents were positively correlated whereas pH was negatively correlated. Soils having low pH, high OM and high clay contents showed higher adsorption. Desorption studies revealed that there was a hysteresis effect in all the soils. Hysteresis coefficient values (ratio of n(ad) and n(des)) varied from 0.09 to 0.45. The study implies that, because of its moderate to high adsorption, flufenacet is likely to persist in soil for some time. However, the possibility of its movement by leaching or surface run off is less. 相似文献
9.
Isoxaflutole, [4-(2-methanesulfonyl-4-trifluoromethylbenzoyl)-5-cyclopropyl isoxazole] is a relatively new pre-emergence herbicide which undergoes rapid conversion to a diketonitrile metabolite in soil. The half-life of isoxaflutole is very short but the half-life of diketonitrile is much longer and hence, diketonitrile remains for a extended period of time in soil. Sorption-desorption studies were conducted with five soils varying in physical and chemical properties. The batch equilibration technique was used for the sorption experiments, while completely mixed batch reactor systems with the decant and refill method was used for the desorption experiments. Four subsequent desorptions were examined after the sorption process in each soil with an equilibration period of seven days. An apparent sorption-desorption hysteresis was observed in all five soils. Organic matter content and the clay content of the soils were the two determining factors for hysteresis. In soils with high organic matter content, the sorption-desorption hysteresis was mainly governed by organic matter content, but in soils with low organic matter clay content played an important role. With the exception of the Chelsea soil, which had a very high organic matter content (57.4%), all other soils exhibited a high correlation between the clay content and hysteresis index (HI) values calculated at 0.75 ( r 2 = 0.960), 25 ( r 2 = 0.934) and 150 mg L−1 ( r 2 = 0.928). In conclusion, the potential for leaching through soil and crop injury due to isoxaflutole and its metabolite would decrease as soil organic matter and clay content increases. 相似文献
10.
研究建立了烟叶及土壤环境中嘧肽霉素残留的高效液相色谱(HPLC)检测方法:鲜烟叶样品采用V(乙腈):V(水)=19:1的混合溶剂提取,干烟叶及土壤样品采用V(乙腈):V(水)=17:3的混合溶剂提取,经PEP-SPE固相萃取柱净化,HPLC检测。结果表明:在0.05～2 mg/kg添加水平下,嘧肽霉素在鲜烟叶、干烟叶和土壤中的平均回收率分别为82.7%～89.6%、78.7%～81.5%和79.6%～97.8%,相对标准偏差(RSD)分别为4.9%～5.7%、2.1%～5.8%和3.2%～6.1%;烟叶和土壤中嘧肽霉素的最小检出量(LOD)均为0.05 mg/kg。采用所建立的方法测定了田间不同施药剂量、施药次数和采收时间下烟叶及土壤样品中嘧肽霉素的消解动态及最终残留。结果表明:嘧肽霉素在鲜烟叶和土壤中的半衰期分别为3.4～5.1 d和1.3～3.1 d;于烟草现蕾-成熟期,以2%嘧肽霉素水剂按有效成分28.2～42.3 g/hm2的剂量施药2～3次,距末次施药后7、14和21 d,烟叶及土壤中嘧肽霉素的残留量均低于LOD值(0.05 mg/kg)。 相似文献
11.
Sorption of added zinc to irrigated soils in arid regions is an important process that may control the availability of zinc to growing plants . Two soil surface samples varying in clay , organic matter , and calcium carbonate content were selected from central and southwestern regions of Saudi Arabia and prepared in order to give different initial moisture contents ranging from air dried to 100 % of field capacity . The sorption experiment was conducted using Zn concentrations ranging from 5 to 25 mg L 1, prepared from ZnSO4 either in distilled water or in solutions containing 75 mg L 1 dissolved organic carbon (DOC). Results indicate that the amount of Zn sorbed in the presence of DOC was relatively high compared with the absence of DOC and Zn retention was strongly affected by the initial soil moisture content . Also , equilibrium Zn concentrations were quite low , while Zn retentions were high in all treatments . Data of Zn sorption were described by the Freundlich isotherm , and two linear portions were found in most cases . In the absence of DOC , retentions of added Zn were controlled by the available exchange sites and / or the precipitation of Zn as sparingly soluble forms. Zn ions in the presence of DOC were able to form soluble - Zn organic complexes that adsorb on the soil surfaces . The extent of such behavior was related to the variations in clay , organic matter , and calcium carbonate contents as well as the initial moisture of the soil . Results indicate that addition of DOC reduces the amount of extractable Zn from either soil Zn or the sorbed Zn by ammonium bicarbonate diethylenetriamine pentaacetic acid ( AB DTPA ). More than 80 % of the sorbed Zn was extracted by AB-DTPA , and the percentage of extracted / sorbed Zn decreased with the increase in sorbed Zn . The obtained results give evidence that initial moisture content and addition of DOC reduce the extractability of applied inorganic Zn by AB-DTPA extract in arid soils. 相似文献
12.
磺草酮在土壤中的淋溶特性研究 总被引：4，自引：4，他引：0
基于所建立的土壤中磺草酮残留的超高效液相色谱-串联质谱分析方法,通过土壤薄层层析试验研究了磺草酮在中国3种典型土壤中的淋溶特性。结果表明:添加水平为1和10 mg/kg时,磺草酮在土壤中的添加回收率为80%~104%,相对标准偏差为1.2%~8.1%,最低检测浓度为0.1 mg/kg。磺草酮在河北潮土、湖南红土和吉林黑土中的比移值(Rf)分别为0.563、0.101和0.422,其在潮土和黑土中的移动性为中等,在红土中为不易移动;磺草酮在土壤中的淋溶特性与土壤理化性质密切相关,主要影响因素是土壤p H值及黏粒组分含量。 相似文献
13.
建立了基质固相分散-高效液相色谱法(MSPD-HPLC)测定2,4-二氯苯酚(2,4-DCP)和2-甲基-4-氯苯酚(4-C-2-M P)在3种不同类型土壤中残留量的分析方法。土壤样品加入硅胶研匀后,加入2.0 m L蒸馏水使其失活,装入层析柱,用二氯甲烷洗脱。向洗脱液中加入0.5 m L乙二醇,减压浓缩并定容至1.0 m L,HPLC测定。结果表明:在0.01~2.5 mg/kg添加水平下,3种土壤中两种待测物的平均回收率在90%~118%之间,相对标准偏差(RSD)在0.1%~8.5%之间;检测限(LOD)在2~3μg/kg之间,定量限(LOQ)均为0.01 mg/kg。与经典的固-液萃取法(SLE)相比,MSPD法对2,4-DCP和4-C-2-MP的提取回收率较高。通过MSPD-HPLC法测定不同老化时间土壤样品中两待测物的回收率,验证了该方法的实用性。该法操作简单、溶剂用量少、分析时间短,适合用于土壤中2,4-DCP和4-C-2-MP残留量的检测。 相似文献
14.
石灰性土壤硒含量与小麦籽粒硒相关性研究 总被引：2，自引：0，他引：2
对新疆不同地区的39个小麦田耕层土壤及籽粒进行调查取样,研究土壤的全硒、有效硒含量与小麦籽粒硒含量的相关性及土壤硒含量的影响因素。结果表明:土壤全硒含量在0.144~1.153 mg·kg-1之间,其中10%属于少硒土壤(0.125~0.175 mg·kg-1),49%属于足硒土壤(0.175~0.450 mg·kg-1),41%属于富硒土壤(0.450~2.000 mg·kg-1),土壤硒的活化率平均为25.11%;小麦籽粒全硒含量在0.004~0.055 mg·kg-1之间,达到国家谷物类食品富硒标准(0.040~3.000 mg·kg-1)的仅有8%,92%小麦籽粒硒含量低于国家谷物类食品富硒标准,由此可知土壤全硒含量与小麦籽粒硒含量无相关性,而土壤有效硒与籽粒硒含量呈极显著正相关,所以要充分利用富硒土壤生产富硒小麦就必须提高土壤中硒的有效性;土壤有效硒与土壤p H值呈极显著正相关,因此在实际生产中可以通过改善土壤条件的方法来提高土壤硒的有效性,从而提高小麦籽粒中硒的含量;土壤全硒含量随土壤质地粘重程度的增加而增加。 相似文献
15.
Understanding the status and distribution of the micronutrient Zn in soils is important for managing plant growth and preventing soil pollution for agricultural irrigation systems in arid and semi-arid regions.In this study,a total of 195 soil samples from five soil layers(0–20,20–40,40–60,60–80 and 80–100 cm) in the three land-use types(wasteland,forestland and cropland) after long-term agricultural fertilization and irrigation with Yellow River water were collected in the middle of the Hetao oasis,i.e.the Yongji irrigation sub-oasis.We analyzed the vertical and spatial distributions of Zn content and its relationship with soil properties to determine whether differences of Zn content existed in the soil profiles.The results revealed that the mean content of Zn was 107 mg/kg,1.9 times higher than the background value(55.7 mg/kg) of the Hetao oasis and much lower than the secondary standard value(300 mg/kg) of the Chinese Environmental Quality Standard for Soils when p H7.5.Soil Zn contents were not significantly different and the coefficients of variation of Zn contents were less than 50% in the five soil layers.Soil Zn content was similar from southern to northern parts but increased from western to eastern parts in the sub-oasis.Soil Zn contents did not differ significantly among the three land-use types,but soil total nitrogen(TN) contents were significantly higher in the agriculturally managed forestland and cropland than in the wasteland(P0.05).Zn was significantly and positively correlated with TN(F=36.6,P0.001).The use of fertilizers may increase the content of Zn in soils,but flooding irrigation may minimize the differences in the spatial distribution of soil Zn content in the whole sub-oasis.This research is of important value for soil pollution control and sustainable land use management in arid and semi-arid regions. 相似文献
16.
柱前衍生高效液相色谱-串联质谱法测定土壤中草甘膦及其主要代谢物氨甲基膦酸 总被引：2，自引：0，他引：2
建立了土壤中草甘膦及其主要代谢物氨甲基膦酸高效液相色谱-串联质谱(HPLC-MS/M S)残留检测方法。样品经0.6 mol/L的氢氧化钾溶液提取、C18固相萃取柱过滤净化、9-芴基甲基三氯甲烷(FMOC-Cl)柱前衍生,以乙腈和5 mmol/L的乙酸铵为流动相,C18反相色谱梯度洗脱,电喷雾负离子多反应监测模式(MRM)HPLC-MS/MS检测。结果表明:草甘膦和氨甲基膦酸在1.6~200μg/L范围内线性关系良好,检出限(以信噪比S/N=3计)分别为0.80和0.94μg/kg,定量限(以S/N=10计)分别为2.6和3.0μg/kg;不同类型土壤样品中两种目标物3个水平的平均添加回收率在84%~104%之间,相对标准偏差(RSD)为2.8%~7.5%。应用本方法对部分供试土壤样品进行分析,结果发现所检样品中草甘膦和氨甲基膦酸的检出率较高,分别为38.9%和61.1%,两种物质土壤残留行为较为普遍。 相似文献
17.
建立了采用气相色谱-电子捕获检测器(GC-ECD)测定柑桔和土壤中苯丁锡残留量的分析方法。样品经乙腈提取,浓盐酸衍生化,中性氧化铝柱净化。结果表明:在0.5~5.0 mg/kg添加水平范围内,苯丁锡的平均添加回收率为92% ~98%,相对标准偏差(RSD)为5.8% ~8.7%(n=5)。方法的最小检出量(MDL)为1×10-10g,苯丁锡在桔肉、桔皮、全果和土壤4种基质中的定量限(LOQ)均为0.5 mg/kg。该方法杂质干扰少,准确性及灵敏度满足农药残留检测要求,对检测硬件要求低,适用于柑桔和土壤中苯丁锡残留的分析。消解动态试验结果表明,苯丁锡在柑桔和土壤中的消解半衰期分别为9~14 d和9~11 d,属易降解农药。 相似文献
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施用7%草甘膦水剂对土壤盐化和碱化的影响 总被引：2，自引：0，他引：2
通过室内盆栽模拟实验,研究了5种浓度的7%草甘膦水剂对土壤盐化和碱化的影响。结果表明,施药后土壤盐度(用电导率表示)、钠碱化度(ESP)、钠吸附比(SAR)、总碱度及pH值都明显增大,且随施药次数的增加,上述各项盐化和碱化指标不断增大;每次施药后,土壤的各项盐化和碱化指标都随施药浓度的升高呈增大趋势。6次施用0.352 g/L的7%草甘膦水剂后,土壤的电导率由施药前的1 010增加为2 460 μS/cm,ESP由2.247％增加为7.983％,SAR由1.576增加为4.305,总碱度由1.443 mmol/L增加为4.485 mmol/L,pH值由6.92变为7.89。虽然土壤各项盐化和碱化指标的变化都还在非盐化和非碱化土范围内,但有盐化和碱化的趋势。 相似文献
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丙环唑在香蕉和土壤中的消解动态及残留安全性评价 总被引：4，自引：0，他引：4
采用田间试验方法研究丙环唑在香蕉和土壤中的残留动态。超高效液相色谱-串联四极杆液质联用法进行(UPLC-MS/MS)定量定性分析。丙环唑在香蕉中的平均回收率为81.9%～100.2%;在香蕉全果中的平均回收率为72.8%～103.6%;在土壤中的平均回收率为81.9%～94.6%。动态结果表明:丙环唑在香蕉全果中比在土壤中消解快,其消解半衰期分在香蕉全果和土壤中分别为13.9d和23.3d。在香蕉上按照推荐剂量最多施药2次,采收期距最后一次施药40d,香蕉果肉中丙环唑残留量小于0.011mg/kg。低于中国规定的最高残留限量(MRL,0.1mg/kg),说明该药为低残留、易消解农药。 相似文献