水产品等食品中磺胺类抗生素残留分析与预处理方法的研究进展

对水产品等食品中磺胺类抗生素常用的分析方法和预处理方法进行了综述,归纳和比较了毛细管电泳法、微生物方法、液相色谱-质谱法、免疫法、气相色谱法、分光光度法、高效液相色谱法等特点。其中高效液相色谱法由于操作简便、快速、灵敏、准确的特点,是当前检测磺胺类抗生素的主要方法。同时,对包括固相萃取、分子印迹等预处理方法进行了综述。     

高效液相色谱-串联质谱法检测水产品中三聚氰胺残留的比较研究

该研究利用高效液相色谱．串联质谱法（LC—MS／MS）检测水产品中的三聚氰胺,分别比较C18柱、氰基柱（CN）和强阳离子交换与反相C18混合填料柱（CR）3种色谱柱及其相对应的流动相对三聚氰胺的保留和分离效果。结果显示,以甲醇和5mmol的挥发性离子对试剂全氟庚酸作为流动相,采用梯度洗脱,三聚氰胺在C18柱中能得到较好地保留和分离。该研究拓宽了C18柱在药物残留分析中的应用范围。方法成本低、灵敏度高、稳定性和重现性良好,适用于水产品中三聚氰胺的残留检测。     

Separation of fine organic particles by a low-pressure hydrocyclone (LPH)

The separation performance of a low-pressure hydrocyclone was tested using fine organic particles from 1 to 700 μm. The dimensions of the low-pressure hydrocyclone were an inflow diameter of 30 mm, a cylinder length of 575 mm, an overflow diameter of 60 mm, an underflow diameter of 50 mm, a cylinder diameter of 335 mm and a cone angle of 68°. The low-pressure hydrocyclone was operated with a lower inlet pressure (average 1.38–5.56 kPa) that could be maintained under water level differences that ranged from 17.5 to 53.5 cm between the water surface of the feeding mass cylinder and the middle of the inlet pipe of the low-pressure hydrocyclone. By varying the inflow rate, underflow ratio and feed concentration, the separation performance of the low-pressure hydrocyclone was affected. The separation performances were determined from total separation efficiency and grade efficiency. Separation performances were determined according to the different inflow rates of 400, 600, 800 and 1000 ml s⁻¹ and their respective underflow ratios that ranged from 5% to 30%. The maximum total separation efficiencies for each inflow rate were 41%, 46% and 46% at 400, 800 and 1000 ml s⁻¹ inflow rates, respectively, and at underflow rates of 30% of the inflow rates. In addition, a total separation efficiency of 46% was employed at 600 ml s⁻¹ of inflow rate and with an underflow rate of 25% its inflow rate. As the feed concentration increased from 25 to 150 mg l⁻¹, the separation performances were gradually decreased. For the fine particles ranging 1–200 μm, the grade efficiency was higher at the higher inflow rate (higher than 600 ml s⁻¹) and higher underflow rate. However, for the coarse particles ranging 400–700 μm, the grade efficiency was higher at the lower inflow rate (lower than 600 ml s⁻¹) and higher underflow rate. The cut-point (d₅₀) values ranged from 30 to 200 μm for a feed size range of 1–700 μm. The Response Surface Method (RSM) model predicted an optimum operating inflow rate and underflow ratio of 721 ml s⁻¹ of inflow rate and 30%, respectively, for the low-pressure hydrocyclone at a maximum total separation efficiency. Based on these findings, further design and operating adaptation of low-pressure hydrocyclones used for fine solids removal in recirculating aquaculture systems is expected.     

液相色谱-串联质谱法测定水产品中孔雀石绿的残留量

建立了液相色谱-串联质谱测定水产品中孔雀石绿及其代谢物残留的检测方法。样品经乙酸铵盐溶液和乙腈提取,经二氯甲烷萃取,PRS阳离子交换柱净化,然后选用电喷雾离子源,在正离子、多反应监测方式模式下进行定性,以内标法进行定量。方法的检出限为0.10μg·kg-1,工作曲线的线性范围为0.10~4.00μg·kg-1。在添加浓度为0.10~4.00μg·kg-1的范围内,孔雀石绿和隐色孔雀石绿的平均回收率均分别为83.4%和95.0%,相对标准偏差分别为6.23%和6.74%。     

醉鱼糟制过程中酒糟液中的微生物群落

为探讨醉鱼糟制过程中酒糟液微生物群落多样性,本实验以大黄鱼为原料,用传统糟制工艺制作醉鱼,采用Illumina HiSeq2500高通量测序技术对醉鱼酒糟液菌群进行分析。结果显示,糟制过程中不同用盐量(2%、5%和10%)大黄鱼pH值在糟制前5 d或10 d稍有上升后逐渐降低,而TVB-N值在糟制期间逐渐下降,糟制30 d后的TVB-N值均低于30 mg/100 g,其中5%用盐量组最低;5%用盐量组在不同鱼糟比(1:1、1:1.5和1:2)下,大黄鱼pH和TVB-N值变化规律基本一致,说明糟制过程中醉鱼品质较稳定。5%用盐量组醉鱼酒糟液微生物高通量测序结果显示,鱼糟比为1:2的酒糟液Chao指数最大(167),表明物种丰度最高;鱼糟比为1:1的酒糟液Shannon指数最大(2.75),Simpson指数最小(0.109),表明细菌多样性最高;酒糟液涉及细菌17个门和1个未分类菌门,143个属,变形菌门、蓝细菌门和厚壁菌门是优势菌门,其中变形菌门占绝对优势;弧菌属、Chloroplast norank和肠杆菌属是优势菌属,发酵前期弧菌属占绝对优势。研究结果为醉鱼酒糟液微生物群落多样性研究提供理论依据,为控制糟制水产品卫生安全提供参考。     

厚壁轮枝菌摇瓶液体发酵培养的研究

厚壁轮枝菌对根结线虫虫卵有很强的寄生力,是线虫的生防菌,本文对其最适培养条件进行了研究.每12 h对其产孢情况进行跟踪,探讨了不同C、N源,初始pH值,无机盐对其产孢量的影响,确定了适宜的培养条件及发酵终止时间.结果显示,28 ℃下,在160 r·min-1 摇床上,以500 mL三角瓶200 mL的装量进行液体培养,筛选出的最佳复合培养基配方为:葡萄糖20 g·L-1,玉米粉20 g·L-1, 黄豆粉20 g·L-1,KH2PO4 0.5 g·L-1 ,MgSO4·7 H2O 0.5 g·L-1.最佳pH值范围5.0～7.0,最适发酵终止时间120～144 h.     

弧型齿残膜捡拾滚筒捡膜的机理

对弧型齿残膜清理滚筒捡膜齿的轴向排列、滚筒转速、捡膜齿运动轨迹和各相关参数进行分析研究,初步找出弧型捡膜齿满足要求的排列布置、滚筒转速和合理的入土深度,确定了残膜回收机具的运动参数λ范围,为残膜清理滚筒的设计提供了理论依据。试验表明,所设计的残膜回收机具运动参数是合理的,在保证膜土分离效果好和较高残膜捡拾率的前提下可显著提高工作效率。     

底泥中除草剂灭草松残留量的测定

[目的]利用超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS),检测底泥中灭草松除草剂残留。[方法]底泥样品经索氏提取,C_(18)固相萃取柱净化后,在多反应监测(MRM)负离子电喷雾模式下进行UPLC-MS/MS分析。色谱柱为BEH C_(18)反相柱(50.0 mm×2.1 mm,1.7μm),流动相为梯度变化的乙腈和2 mmol/L乙酸铵+0.1%甲酸水溶液。[结果]灭草松的检出限(S/N≥3)为0.3μg/kg,在各自的考察浓度范围内线性关系良好(r≥0.998);在1.0~20.0μg/kg添加水平内,平均加标回收率在82%~116%之间,RSD为3.6%~9.7%。[结论]利用该方法可以实现底泥中灭草松除草剂残留量的高灵敏度检测。     

表面油流法显示螺旋离心泵内部流动的研究

对螺旋离心泵叶轮、进水节和进水节与蜗壳交界处的部分端面做了表面油膜、油点试验。通过流谱分析，揭示了表面奇点、分离线与再附着线等流动特征，研究了螺旋离心泵内部流动规律，进而提出了改进螺旋离心泵结构的设想。     

用超临界CO2脱除绿茶浓缩液中咖啡碱的工艺研究

对绿茶浓缩液中咖啡碱的超临界CO₂萃取工艺进行了研究，通过4因素正交试验探讨了浓缩液的浓度、操作压强、操作温度、萃取时间对咖啡碱脱除率的影响。结果表明，超临界CO₂萃取技术可以有效地脱除绿茶浓缩液中大部分的咖啡碱，在此基础上完成了用超临界CO₂脱除绿茶浓缩液中咖啡碱的连续作业试验，从而获得了加工脱咖啡碱绿茶浓缩液或速溶绿茶的新工艺。