加快发展亚氨基二乙酸

介绍了亚氨基二乙酸的用途,市场及国内开发生产情况,提出要加快开发天津大学新工艺的进程,对氢氰酸工艺深入研究,以充分利用氢氰酸。并建议新建装置以3000t/a以上为宜。     

IDA法草甘膦废液电渗析脱盐的研究

采用电渗析法在不同溶液pH值、流量、浓度差下脱除草甘膦废液中的硫酸铵,处理后的草甘膦废液可以通过膜分离设备回收利用.     

Alfalfa containing the glyphosate-tolerant trait has no effect on feed intake, milk composition, or milk production of dairy cattle

The objective of this experiment was to assess if feeding glyphosate-tolerant alfalfa affects feed intake, milk composition, or milk production of dairy cows. One alfalfa (Medicago sativa), variety expressing the CP4 EPSPS protein and grown in southeastern Washington State was harvested at the late vegetative stage as hay. Three commercial conventional varieties of alfalfa hay of similar nutrient composition and harvested in the same geographic region were fed to cows as controls. The commercial hays were selected to be similar in crude protein [18% of dry matter (DM)] and neutral detergent fiber (40% of DM) to the glyphosate-tolerant hay. Sixteen multiparous Holstein cows were fed diets containing alfalfa hay (39.7% of diet DM) from either the glyphosate-tolerant alfalfa, or 1 of the 3 conventional varieties. Diets contained at least 15.7% crude protein and 29% neutral detergent fiber. Experimental design was a replicated 4 × 4 Latin square. Periods were 28 d and feed intake, milk yield, and milk composition were summarized over the last 14 d of each period. Daily milk yield (38.0 kg) and 4% fat-corrected milk (34.7 kg) were not affected by treatment. Milk fat (3.44%) and milk true protein (2.98%) were also not affected by source of hay. Milk lactose (4.72%) and soldis-not-fat (8.5%) did not differ due to treatment. Dry matter intake was similar across treatments (24.4 kg/d). These results are consistent with data from feeding trials with other glyphosate-tolerant crops and previously reported compositional comparisons of glyphosate-tolerant alfalfa with controls. Milk production, milk composition, feed intake, and feed efficiency were not affected by feeding diets that contained nearly 40% glyphosate-tolerant alfalfa hay to lactating dairy cows.     

离子色谱法测定食品中草铵膦、草甘膦和 氨甲基膦酸的残留

目的建立一种简单、快捷、同时测定食品中草铵膦、草甘膦、氨甲基膦酸残留量的离子色谱分析方法。方法样品用水提取后使用乙腈沉淀氨基酸和蛋白质,离心后取上清液依次过Dionex OnGuardⅡRP柱和Dionex OnGuardⅡAg/H柱,流出液经IonPac AS11-HC离子色谱柱(含AG11-HC保护住)分离,用KOH淋洗液自动发生器(EG)进行梯度淋洗,抑制器采用外加水模式,电导检测器检测。结果结果表明草甘膦和草铵膦在0.02~6.25 mg/L、氨甲基膦酸在2.00~62.5 mg/L范围内线性关系良好,相关系数均大于0.999,Gly、Gluf和AMPA的方法检出限分为0.047、0.033和0.520 mg/kg,定量限分为0.16、0.11和1.73 mg/kg,回收率为80.1%~109%,日内精密度(n=6)为0.91%~12.5%,日间精密度(m=5)小于10.0%。结论该方法具有净化效果好、定量准确、灵敏快速的特点,适用于食品中草铵膦、草甘膦、氨甲基膦酸残留量的检测确证,能达到GB 2763-2014的检测要求。     

柱前衍生-固相萃取-高效液相色谱荧光法 测定蔬菜中草甘膦

目的建立快速、准确的蔬菜中草甘膦的柱前衍生-固相萃取-高效液相色谱荧光测定方法。方法蔬菜提取液样经衍生后经固相萃取,过C_(18)色谱柱,以甲醇-水(70:30,V:V)为流动相,流速1.0 mL/min,柱温为35℃,荧光检测激发波长为265 nm,发射波长为3 15 nm。结果草甘膦的加标回收率在89.2%~99.2%范围,其相对标准偏差均5.0%,在0.5~20.0 ng/mL范围呈现良好的线性,其回归系数0.999,最低定量检出限(LOQ)为0.02 mg/kg。结论本方法回收率高,净化效果好,杂质干扰少,可满足蔬菜中痕量草甘膦的残留检测要求。     

草甘膦人工抗原的制备及兔源多抗的ELISA鉴定

采用1-(3-二甲氨基丙基)-3-乙基碳二亚胺(1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride,EDC)法和戊二醛(glutaraldehyde,GA)法,合成了草甘膦(N-(phosphonomethyl)glycine,PMG)人工抗原,通过免疫制备高敏感性、特异性的兔PMG多克隆抗血清并进行鉴定。将PMG分别与牛血清白蛋白(bovine serum albumin,BSA)和鸡卵清白蛋白(ovalbumin,OVA)偶联,合成免疫抗原PMG-BSA和包被抗原PMG-OVA。经紫外扫描、十二烷基硫酸钠-聚丙烯酰胺凝胶电泳鉴定后,免疫新西兰大白兔,制备多抗。利用间接酶联免疫吸附(enzyme linked immunosorbent assay,ELISA)方法测定多抗效价,间接竞争ELISA方法测定血清的敏感性和特异性。结果表明,免疫的3只兔血清效价均达1∶104以上,2号兔多抗效果最好,半数抑制浓度(IC50)为30.9μg/m L,且具备良好的特异性。本实验成功合成了PMG人工抗原,并制得了敏感性高、特异性好的兔多抗,为PMG的免疫学快速检测方法的提供参考。     

分散固相萃取/衍生化-高效液相色谱-串联质谱法同时测定水和食品中草甘膦、草铵膦和氨甲基膦酸残留

目的建立高效液相色谱-串联质谱法测定水和食品中草甘膦、草铵膦和氨甲基膦酸的残留量。方法样品经纯水涡旋超声提取,二氯甲烷去除脂肪,C_(18)分散固相萃取净化,(水样)净化液在硼酸盐缓冲液中加入9-芴基甲基三氯甲烷(FMOC-Cl)丙酮溶液进行衍生化2 h以上,经0.22μm微孔滤膜过滤,经CAPCELLCORE C_(18)柱分离,用5 mmol/L乙酸铵溶液和乙腈为流动相梯度洗脱,采用电喷雾负离子多反应监测模式检测,外标法定量。结果草甘膦、草铵膦和氨甲基膦酸在0.5~40μg/L浓度范围内呈良好的线性关系(r0.999),方法定量限为0.5μg/kg。在0.5、5.0和20μg/kg添加水平时,平均回收率为70.1%~104.1%,相对标准偏差为0.6%~8.9%(n=6)。结论该方法分析速度快,净化效果好,杂质干扰小,回收率高,重复性好,适用于水和食品中草甘膦、草铵膦和氨甲基氨酸留量的测定。     

16％草甘膦异丙胺盐水剂对柑桔园杂草的防效研究

草甘膦异丙胺盐是一种灭生性除草剂，具有活性高，见效快，用量少，杀草谱广等特点。对16％草甘膦异丙胺盐水剂进行了柑桔园杂草的防除试验，结果表明，16％草甘膦异丙胺盐水剂对桔园杂草有优良的防治效果，6000mL/hm^2的处理在施药后15-28d的株防效达96．85％～99．39％，鲜重防效达97．50％。     

草甘膦生产中三乙胺回收工艺改进

本文介绍了从草甘膦结晶母液中回收三乙胺的工艺改进。采用中和分层与连续精馏相结合的工艺取代了原有的间歇回收工艺。新工艺的主要优点是回收率高、节能显著、操作简便。     

气相色谱-质谱法测定黑木耳中草甘膦和氨甲基膦酸残留量

目的 采用气相色谱-质谱法建立一种黑木耳中草甘膦和氨甲基膦酸残留的分析方法。方法 干制黑木耳样品经二氯甲烷脱色、水提取、盐酸沉淀蛋白、乙醇沉淀多糖后, 与三氟乙酸酐和七氟丁醇进行衍生化反应, 经气相色谱柱分离后, 在选择离子监测（selected ions monitoring, SIM）模式下进行草甘膦和氨甲基膦酸含量的测定, 外标法定量。结果 干制黑木耳中草甘膦在0.001~0.050 μg/mL浓度范围内呈现良好线性(相关系数R2=0.9993), 表现为弱基质抑制效应, 检出限为0.02 mg/kg, 定量限为0.04 mg/kg, 在0.04、0.08、0.20 mg/kg 3个添加水平下, 平均回收率为82.4%~93.4%, 相对标准偏差为7.8%~9.5%(n=6); 氨甲基膦酸在0.0005~0.050 μg/mL浓度范围内呈现良好线性(相关系数R2=0.9996), 表现为弱基质增强效应, 检出限为0.01 mg/kg, 定量限为0.02 mg/kg, 在0.02、0.08、0.20 mg/kg 3个添加水平下, 平均回收率为85.6%~96.8%, 相对标准偏差为5.7%~9.3%(n=6)。结论 该方法针对干制黑木耳基质, 样品前处理过程简单, 净化除杂效果好且回收率高, 满足农药残留分析实验室对黑木耳中草甘膦和氨甲基膦酸残留的检测要求。