烟草中溴菌腈农药残留检测方法及消解动态

为摸清溴菌腈在烟草中的农药残留消解动态规律及残留特征,建立了QuEchERS前处理和气相色谱-串联质谱(GCMS/MS)检测相结合的烟叶中溴菌腈残留量的分析方法。烟叶经乙腈提取,N-丙基乙二胺吸附剂(PSA)净化,气相色谱-串联质谱法检测。结果表明,在0.01~1.0 mg/kg 3个添加水平下,溴菌腈在鲜烟叶和干烟叶中的平均回收率分别为85.8%~94.5%、83.2%~110.0%,相对标准偏差(RSD)分别为1.4%~10.6%、7.3%~14.1%,定量限(LOQ)均为0.01 mg/kg。利用山东和湖南2年2地的溴菌腈在烟叶中农药残留田间试验样品进行了深入研究,溴菌腈在烟叶中的半衰期7.8~14.9 d;按照162 g.a.i./hm²和243 g.a.i./hm²剂量,分别灌根施药1~2次,末次施药14 d后,溴菌腈在烟叶样品中的最终残留量为0.010~0.13 mg/kg。根据烟草青枯病发病条件、发病时期、农药在烟叶中使用情况及OECD农药残留限量计算结果,建议溴菌腈在烟叶中残留限量为0.2 mg/kg,安全间隔期为14 d。     

Pesticide residue monitoring in Korean agricultural products, 2003–05

Between 2003 and 2005, a total of 11,716 samples were collected and analysed to determine the level of pesticides residues. Multi-residue methods (MRMs) capable of simultaneously determining 250 pesticides were used. Of the 11,716 samples, 89.1% had no detectable residues and 1.7% had violative residues. The detection rates by commodity group were 11.4, 8.6, 0.3, and 0.02% for vegetables, fruit, grain, mushrooms, and the others, respectively. Agricultural products with pesticide residues were pepper, Perilla frutescens, leafy lettuce and spinach in decreasing order. Of the 250 pesticides that were monitored, 70 pesticides were actually found. Procymidone, endosulfan, chlorfenapyr, metalaxyl, and diethofencarb were frequently detected. Of the samples, parsley, Petasites hybridus, Aster scaber and leek had high violative rates of 23.1, 12.6, 8.2, and 7.9%, respectively. From violative samples, procymidone, endosulfan, metalaxyl, diazinon and chlorpyrifos were frequently detected. The violation rates were 1.71, 1.68, and 1.76% in 2003, 2004 and 2005, respectively, and the detection rates were 8.5, 12.0, and 13.3% in 2003, 2004, and 2005, respectively.     

Changes of intramuscular phospholipids and free fatty acids during the processing of Nanjing dry-cured duck

In this study, changes of intramuscular phospholipids and free fatty acids were tracked during the processing of Nanjing dry-cured duck. Phospholipids were identified and quantified by high performance liquid chromatography combined with UV and evaporative light scattering detectors. The types and quantities of free fatty acids and fatty acids derived from phospholipids were analyzed by capillary gas chromatography. The results showed that raw duck meat had high quantities of phosphatidylethanolamine, and phosphatidylcholine (37.95% and 54.07% of total phospholipids, respectively), which contained high percentages of polysaturated fatty acids. The percentages of total phospholipids, phosphatidylethanolamine, and phosphatidylcholine decreased during processing, with a concomitant increase in quantities of free fatty acids. The lipolysis of phospholipids, especially phosphatidylethanolamine is the main contributor to the increase of free fatty acids.     

无溶剂萃取技术在食品中农药残留分析的研究进展

无溶剂萃取技术是一种先进的样品制备与前处理技术,常用的有气相萃取、超临界流体萃取、固相萃取、固相微萃取等方法。本文综述了无溶剂萃取技术的基本原理及在食品中农药残留的研究应用进展。     

工业碱渣生产亚硫酸钠的工艺研究与应用

文章通过对水合肼副产碱渣成份与亚硫酸钠性质的分析,以及碱液对二氧化硫吸收原理的研究,提出了一条利用水合肼副产十水碳酸钠制亚硫酸钠的生产方法,并将研究结果成功应用在工业生产上,具有投资少、成本低、操作方便等优点,为水合肼副碱渣提供了一条可靠的处理途径。     

节能型甲基异丙基酮分离工艺研究

甲基异丙基酮生产中,水与甲基异丙基酮等形成共沸物,文中运用剩余曲线图(RCM)方法对甲基异丙基酮分离过程进行分析研究,根据非均相共沸精馏原理,提出了在丙酮塔中增加油水分离器的方法脱除待分离物系中的水,从而达到节能的目的。文章在Aspen Plus中建立了该节能型甲基异丙基酮分离过程的模拟模型,进行了计算和分析,并加以实验验证,二者比较吻合。结果表明,该分离工艺即节省了设备投资,又降低了分离能耗,并且提高了脱水效率,改善了产品质量,同时还提高了产品收率,所用方法对简化工艺流程起到了积极作用。     

玉米淀粉残渣中油脂的亚临界流体提取与制备生物柴油的研究

研究通过亚临界流体提取技术提取玉米淀粉残渣中的油脂,再将提取出的油脂经过预酯化过程、醇解过程,制备生物柴油。结果表明,在玉米淀粉残渣油脂的亚临界流体提取过程中,适宜条件为提取温度40℃、每次提取时间40 min、料液比1∶2、提取次数3次,在该条件下油脂得率为46.68%;预酯化过程的适宜条件:在真空条件下,反应温度190℃,甘油添加量为理论添加量的175%,催化剂用量为油脂质量的2%,反应时间3 h;经预酯化处理后进一步醇解得到生物柴油,醇解反应的脂肪酸甲酯产率为95.21%。     

正交试验法优化水提紫甘薯色素废渣发酵酒工艺及模糊综合评判模型评价感官质量

以水提紫甘薯色素废渣为主要原料,经发酵工艺制得发酵酒,应用模糊综合评判模型评价发酵酒成品。结果表明,发酵温度、料液比、蔗糖添加量、发酵时间是影响发酵酒的关键因素,采用正交试验L9(34)确定最佳工艺为发酵温度25℃、料液比1:25、蔗糖添加量22%、发酵时间12d。模糊综合评判模型评价结果,9个酒样的感官质量优劣顺序为6#>3#>5#>4#>7#>9#>2#>1#>8#。模糊综合评判结果准确、科学。     

气相色谱法检测茶叶中痕量双甲脒

研究应用气相色谱法测定茶叶中痕量双甲脒残留物的分析方法。对样品预处理的方法进行探索,最终选择出较为理想的提取试剂,并对定量检测条件作了较详细的研究。     

气相色谱串接质谱测定食醋中多组分农药残留含量的方法研究

该研究建立了食醋中多组分农药残留的气相色谱串接质谱（GC-MS/MS）检测法,并成功运用于市售食醋中农药残留的定量 检测。食醋先用氨水中和至中性,再用甲苯/环己烷的混合溶液提取,经石墨化炭黑（GCB）和N-丙基乙二胺（PSA）净化,有机相膜过滤后 进样。样品经DB-5MS柱分离后采用多反应监测（MRM）模式进行检测,外标法定量。目标化合物在一定质量浓度范围内（7.81～125 μg/L） 线性关系良好,相关系数R2均＞0.99。方法的定量限（LOQ）和检出限（LOD）分别为10.0μg/L、5.00μg/L,平均回收率为78.5%～112.0%,相对标准偏差（RSDs）为5.90%～11.40%。该方法简便、快速、准确,已成功应用于市售食醋中农药残留的检测。