Lipase biosensor for tributyrin and pesticide detection

Potentiometric biosensors based on Candida rugosa lipase was described for the detection of organophosphorus pesticide; methyl-parathion and tributyrin. Lipase was immobilized on the glass electrode by means of a gelatin membrane, which is then cross-linked with glutaraldehyde. The principle of the biosensor is based on the measurement of pH variation which was recorded in millivolts due to the enzymatic hydrolysis of tributyrin to butyric acid. For the inhibitor detection, biosensor responses were measured after pesticide treatment, which caused a drop in enzyme activity because of the irreversible inhibition. Reactivation conditions of the reused enzyme electrodes were also investigated by pyridine-2-aldoxime methiodide (2-PAM). The limit of detection for tributyrin was estimated as 93?µM for lipase sensor within the linear range of 65–455?µM.     

气相色谱-三重四极杆串联质谱法快速测定蔬菜水果中129种农药的残留量

采用QuEChERS方法结合气相色谱-串联质谱法(GC-MS/MS)建立了蔬菜、水果中129种农药残留同时检测的分析方法。试样用1%乙酸乙腈均质提取,采用混合型固相分散萃取剂净化后,用GC-MS/MS在多反应离子监测(MRM)模式下进行检测,外标法定量。结果表明,129种药物在一定的含量范围内线性关系良好,相关系数(r2)均大于0.98;不同基质在10 μg/kg添加水平下大部分农药的平均回收率为66.2%～124.7%,相对标准偏差(RSD)为0.9%～24.4%;方法的定量限(LOQ)为0.03～16.7 μg/kg。结果表明,该方法简便快速、灵敏可靠、经济有效,适用于蔬菜、水果中农药多残留的同时快速筛查测定。     

Reliable screening of pesticide residues in maternal and umbilical cord sera by gas chromatography-quadrupole time of flight mass spectrometry

The widespread use of pesticides induces heavy adverse effects on human health,especially for the pregnant women and the newborns.In this study,a screening method has been developed for the determination of multi-pesticides in maternal and umbilical cord sera.All pesticides in sera were collected using solid phase extraction(SPE),and analyzed by gas chromatography-quadrupole time of flight mass spectrometry(GC-QTOF MS).To set up the quality criteria,a database of 50 pesticides was created and the accurate masses of 3 up to 5 representative ions with their intensity ratios were included for each pesticide.In addition,a novel"identification points"(IPs)system relying on the accurate MS1 and MS2 spectra was used to interpret the data for each suspected pesticide.The methodology was then applied to a pair of maternal and umbilical cord sera.A total of six pesticide residues were screened out successfully.In conclusion,GC-QTOF MS combined with an accurate mass database seemed to be one of the most efficient tools for systematic pesticide analysis.     

粮油作物及茶叶中农药多残留检测的前处理技术进展

综述了粮油作物和茶叶中农药多残留检测的前处理技术,包括超临界流体萃取、加速溶剂萃取、搅拌棒吸附萃取、分散固相萃取、固相微萃取和在线凝胶渗透色谱等样品前处理方式,并详细介绍了各种方法的原理、优点及适用范围,可为粮油作物和茶叶中农药多残留检测技术的发展提供参考。     

电动流动分析和酶抑制法测定池塘水中农药残留折合总量

用电动流动分析和酶抑制法测定池塘水中有机磷和氨基甲酸酯农药残留折合总量。电动流动分析系统由一台自制电渗泵和4个电磁切换阀组成,由计算机编程控制。酶抑制法用面粉酯酶,有机磷和氨基甲酸酯农药作酶抑制剂,底物的酶解产物与显色剂反应,用分光光度计在524 nm检测。有机磷和氨基甲酸酯农药的折合浓度对数线性范围为0.02~0.20 mg/L乐果,检出限为0.01 mg/L乐果,每小时可测24个样品。氨基甲酸酯在80℃完全水解,而有机磷部分水解,据此可判断农药类别。     

生晒参、全须生晒参中19种有机氯残留农药的毛细管气相色谱测定

建立了生晒参、全须生晒参中19种有机氯农药残留的毛细管气相色谱分析方法。对样品中六六六的4种异构体、滴滴涕的5种异构体、四氯苯胺、六氯苯、五氯硝基苯、七氯、五氯苯胺、艾氏剂、百菌清、环氧七氯、狄氏剂及异狄氏剂共19种有机氯农药的残留量进行了测定。以石油醚-丙酮混合物作为提取剂,样品采用索氏提取,提取液用弗罗里硅土柱层析净化。采用OV-1701石英毛细管气相色谱柱分离样品,ECD检测器进行检测。在3个水平添加时的回收率(n=5)分别为75.7%~96.1%、78.8%~111.6%和81.7%~115·2%;相对标准偏差分别为2.4%~10.6%、2.1%~9.8%和1.4~10.0%。方法用于生晒参和全须生晒参样品中农药残留的测定,结果满意。     

用于水中有机磷农药检测的离子迁移率谱仪预富集进样方法

建立了检测水中有机磷农药的离子迁移率谱仪预富集进样方法。预富集器由表面覆盖有吸附薄膜的微热板、聚四氟乙烯电路板和管座组成,具有操作简单,无需有机溶剂,自加热,热容小,功耗低等优点。以马拉硫磷检测为例,分析了富集器解吸升温速率和离子迁移率谱仪半透膜温度对检测结果的影响。采用高温短时脉冲加热和低温维持加热相结合的解吸方式,既可形成较高的进样浓度脉冲,又可减少进入漂移管的杂质,有利于提高离子迁移率谱仪检测灵敏度。实验表明:采用所述预富集及两阶段加热解吸进样方法,对水中马拉硫磷的检出限为3.9μg/L,达到了国家标准对水中有机磷检测的要求。     

稻瘟灵单克隆抗体的制备及评价

该文制备了农药稻瘟灵的单克隆抗体,并建立了稻瘟灵的酶联免疫吸附（ELISA）检测方法。在完全保留稻瘟灵结构的基础上从二硫杂环戊烷结构中衍生不同长度的活性手臂制备了2个半抗原,并分别与载体蛋白偶联合成免疫原与包被原。通过小鼠免疫、细胞融合、淘筛、腹水制备等步骤获得特异性识别稻瘟灵的单克隆抗体mAb-DWL。结果显示,基于mAb-DWL构建的间接竞争ELISA法的半抑制浓度（IC50）为55.2 ng/mL,线性范围为4.6～530.2 ng/mL,其与结构类似物的交叉反应可忽略不计。所建立的ELISA方法对蔬菜及粮食等样品的加标回收率为77.2%～116%,可用于实际样品的快速检测。     

高效光催化活性钠米农药制剂的制备

采用钛酸丁酯水解法制备出直径约为20 nm的纳米TiO2,并用钛酸丁酯对其进行改性。研究表明TiO2与硬脂酸事实上通过化学键键合,由亲水性变为亲油性。文中还提出了三种制备TiO2复合纳米农药制剂的方案,并探讨了几种TiO2复合纳米农药制剂在不同条件下的光催化降解率。结果表明,采用钛酸丁酯为原料直接在农药乳油中原位生成的TiO2复合纳米农药制剂与原农药性状保持基本一致,光催化降解率最大。     

中草药中有机磷及氨基甲酸酯类农药残留量的GC-MS测定

气相色谱-质谱法同时测定中草药中多种有机磷及氨基甲酸酯类农药残留量.采用V(乙腈)∶V(丙酮)＝3∶7混合溶剂微波辅助提取,弗罗里硅土和中性氧化铝层析柱净化,气相色谱-质谱(GC-MS)联用检测,农药混标在0.01～1.0 μg/mL范围内线性良好,在0.5、0.1、0.05 μg/mL 3个水平添加平均回收率分别为86.5%～110.6%、81.2%～108.3%和72.9%～122.3%,相对标准偏差分别为2.6%～8.3%、4.6%～9.7%和2.3%～10.7%.