液相色谱-电喷雾电离三级四极杆质谱法测定茶叶中6种烟碱类农药残留

应用液相色谱-电喷雾电离三级四极杆质谱(LC-ESI-MS/MS)方法测定茶叶中呋虫胺、噻虫嗪、噻虫胺、吡虫啉、啶虫咪和噻虫啉烟碱类农药残留.前处理方法包括添加同位素内标吡虫啉-D4,乙腈提取,再用活性碳和Oasis(HLB)固相小柱净化.该方法采用正离子方式,多反应监测每种烟碱类杀虫剂各两对离子进行定性、定量分析.方法在0.01～0.4 mg/kg范围内具有良好的线性关系.实验了3个添加水平0.02、0.04和0.2 mg/kg,回收率范围为80.1%～106.1%;相对标准偏差小于9.7%;方法检出限(LOQ)均为0.02 mg/kg.本方法简便、快速、准确,各项技术指标满足国内外法规的要求,可用于茶叶样品中烟碱类农药残留的确证检测.     

高效液相色谱-电喷雾串联质谱法快速测定纺织品中苯氧羧酸类除草剂残留量

建立了纺织品中7种苯氧羧酸类除草剂的高效液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)快速检测方法.样品经甲酸酸化的丙酮溶液超声提取两次,无需其它净化过程.液相色谱使用C18反相色谱柱,流动相为醋酸铵水溶液和甲醇,在梯度条件下分析.在选择反应检测(SRM)负离子模式下进行质谱信号采集,采用两对同位素离子对进行定性和定量分析.选取3种有代表性的纺织品进行方法检出限(LOD)、定量限(LOQ)、线性、回收率和精密度的验证.方法的LOQ为 0.9～2.4 μg/kg; 回收率为85%～106%; 相对标准偏差为2%～11%.本方法简便、有效、可靠、灵敏,能够满足国际生态纺织品标准(Oeko-Tex Standard 100)的限量要求,适用于纺织品中苯氧羧酸类除草剂的日常检测及确证.     

用于农药残留检测的酶生物传感器

酶生物传感器在农药残留检测方面具有传统检测方法不可比拟的优势.本文介绍了胆碱酯酶和有机磷水解酶在生物传感器中的应用,重点介绍了用于有机磷等农药残留分析的酶生物传感器的种类和研究现状,讨论了几种酶固定化方法存在的优势和局限,指出了目前研究需解决的问题并展望了未来的发展方向.     

加速溶剂萃取-凝胶渗透色谱净化-气相色谱快速分析动物源性食品中残留的多种有机磷农药

建立了动物源性食品猪肉、牛肉、鸡肉及鱼肉中36种有机磷农药残留的快速分析方法。以乙腈作为溶剂,对试样采用加速溶剂萃取仪萃取,自动凝胶渗透色谱仪净化预处理,N-丙基乙二胺(PSA)填料再净化,毛细管气相色谱法分离,火焰光度检测器(磷型)检测,内标法定量。该方法分离效果良好,重现性好,灵敏度、精密度高,杂质干扰少。36种有机磷农药的检测限(LOD)为0.0012 mg/kg(乙拌磷)～0.014 mg/kg(吡唑硫磷),定量限(LOQ)为0.004 mg/kg(乙拌磷)～0.047 mg/kg(吡唑硫磷)。当试样中有机磷农药的添加浓度分别为0.05,0.1,0.2 mg/kg时,回收率为58.2%～106.3%。方法的最低检测限和添加回收率均符合农药残留分析的要求。     

毛细管区带电泳技术快速分离检测爆炸残留物中的无机离子

利用间接紫外毛细管区带电泳方法完成了对爆炸残留物中7种无机离子(K+,NH+4,NO-2,NO-3,SO2-4,ClO-3,ClO-4)的分离检测。阳离子测定采用的缓冲体系为10 mmol/L吡啶（pH 4.5）-3 mmol/L冠醚,K+和NH+4在2.6 min内达到基线分离,检出限分别为0.25 mg/L和0.10 mg/L(S/N=3)。阴离子测定采用的缓冲体系为40 mmol/L硼酸-1.8 mmol/L重铬酸钾-2 mmol/L硼酸钠（pH 8.6）,氢氧化四甲铵为电渗流改性剂,5种阴离子在4.6 min内达到基线分离,检出限为0.10～1.85 mg/L。该方法已成功地应用于实际爆炸物样品种类的判定分析,取得了很好的结果。     

Evaluation of the aerobic composting process of winery and distillery residues by thermal methods

The possibility of using thermal analysis for a quick characterization of chemical changes was tested in the organic matter from composting materials. Differential thermal analysis (DTA), thermogravimetry (TG) and the first derivative of the TG (DTG) were calculated in oxidizing conditions on compost samples obtained from three composting piles. The composting piles were made by mixing winery and distillery residues with sewage sludge (pile 1), with cow manure (pile 2) and hen droppings (pile 3). The temperature values in the pile 1 showed a different evolution during the thermophilic stage of the composting process in relation to the piles 2 and 3. The thermophilic stage for pile 1 was 17 days, meanwhile for the piles 2 and 3 were around 80 and 110 days, respectively, and probably pile 1 was not well composted. The curves of ion current of CO₂ have been recorded in order to shed light on changes occurring in organic matter during composting. Particularly DTG curves allowed us to distinguish between well (piles 2 and 3) and poor (pile 1) stabilized organic matter. The energy released was calculated for each sample by integrating the DTA curves and these results are agreed with the previous hypothesis. Information deriving from weight losses, registered by the TG and DTG curves, enables to follow the evolution state of the organic matter and therefore changes in its stability. These data could determine the final point of the composting process of winery and distillery residues and then reduce the time for compost harvest.     

浅谈黄原胶及其在农药制剂加工中的应用

黄原胶是极具发展潜力的生物多糖,独特的分子结构使其具有良好的增稠、乳化和稳定作用,已被广泛应用于日用化工、石油开采、纺织印染、食品、医药、涂料、农药等众多工业领域,拥有广阔的市场前景。本文对黄原胶的结构、特性、生产工艺以及主要应用领域等进行了简单综述,总结了黄原胶在农药制剂加工中的应用现状,指出黄原胶优越的流变特性对悬浮剂、水乳剂、悬乳剂等农药制剂悬浮稳定性的提高具有重大意义,最后展望了黄原胶未来的发展前景。     

Tests for standardized generalized variances of multivariate normal populations of possibly different dimensions

In many practical problems, one needs to compare variabilities of several multidimensional populations. The concept of standardized generalized variance (SGV) is introduced as an extension of the concept of GV. Considering multivariate normal populations of possibly different dimensions and general covariance matrices, LRTs are derived for SGVs. The criteria turn out to be elegant multivariate analogs to those for tests for variances in the univariate cases. The null and nonnull distributions of the test criteria are deducdd in computable forms in terms of Special Functions, e.g., Pincherle'sH-function, by exploiting the theory of calculus of residues (Mathai and Saxena,Ann. Math. Statist.40, 1439–1448).     

农药丁吡吗啉与腐殖酸作用机理探讨

探讨农药丁吡吗啉与腐殖酸的作用机理, 可进一步了解农药在土壤中腐殖酸催化下降解的行为过程。将市售腐殖酸进行逐级分离,获得黄腐酸、棕腐酸和黑腐酸的固态或溶液状态,而后分别与农药丁吡吗啉进行作用,利用红外,荧光两种分析方法对其作用机理进行了解释。结果表明,三组分与丁吡吗啉之间广泛存在范德华力、次级键等弱作用力。黄腐酸与丁吡吗啉之间存在氢键和电荷转移吸附等作用力,棕腐酸与丁吡吗啉存在电荷转移吸附等作用力,黑腐酸与丁吡吗啉之间的作用力最弱,即依照黄腐酸、棕腐酸、黑腐酸三组分平均分子量依次递增的顺序,与农药丁吡吗啉之间的作用力依次降低。     

Identification of functionally key residues in maltose transporter with an elastic network model-based thermodynamic method

Periplasmic binding protein-dependent maltose transport system (MBP-MalFGK₂) of Escherichia coli, an important member of the Adenosine triphosphate-binding cassette transporter superfamily, is in charge of the transportation of maltoses across cellular membrane. Studies have shown that this transport processes are activated by the binding of maltose and are accompanied by large-scale cooperative movements between different domains which are mediated by a network of important residues related to signal transduction and allosteric regulation. In this paper, the functionally crucial residues and long-range allosteric pathway of the regulation of the system by substrate were identified by utilising a coarse-grained thermodynamic method proposed by our group. The residues whose perturbations markedly change the binding free energy between maltoses and MBP-MalFGK₂ were considered to be key residues. In result, the key residues in 62 clusters distributed in different subdomains were identified successfully, and the results from our calculation are highly consistent with experimental and theoretical observations. Furthermore, we explored the long-range cooperation within the transporter. These studies will help us better understand the physical mechanism of the effects of the maltose on MBP-MalFGK₂ by long-range allosteric modulation.