SPME-GC-NPD法测定肉制品中挥发性N-亚硝胺

改进3种N-亚硝胺(N-亚硝基二乙胺,NDEA;N-亚硝基二甲胺,NDMA;N-亚硝基吡咯烷,NPYR)的测定方法。以固相微萃取(SPME)为样品萃取方式,配备氮磷检测器的气相色谱仪(GC-NPD)为检测工具,研究3种N-亚硝胺(NDEA、NDMA、NPYR)的测定方法。以PDMS/DVB/CAR为萃取头,萃取温度50℃、搅拌速度400 r/min、萃取时间30 min、盐离子浓度0.20 g/m L时NDEA能得到最大的萃取面积。对3种N-亚硝胺的线性分析得出,NDEA的测定在10 ng/m L~100 ng/m L时线性关系为0.994;NDMA在10 ng/m L~100 ng/m L时的线性关系为0.912;NPYR在0~10 ng/m L时没有表现出明显线性关系。采用SPME,结合GC-NPD测定N-亚硝胺的方法,对NDEA的测定灵敏度最高,RSD为6.7%,加标回收率为89.7%,最低检出限(LOD)0.67 ng/m L,可以满足肉制品中NDEA的定量测定。     

肉制品中9种N-亚硝胺测定方法的建立

建立超声波提取-固相萃取-气相色谱-氮磷检测(UE-SPE-GC-NPD)和超声波提取-固相萃取-液相色谱-紫外检测(UE-SPE-HPLC-UV)肉制品中9种N-亚硝胺的方法。选取二氯甲烷作为提取试剂,探讨萃取时间、有机溶剂用量和萃取功率对提取效果的影响,比较C18、中性氧化铝和活性炭3种固相萃取柱对超声波提取的目标物的净化作用。结果表明:样品经40 mL二氯甲烷在400 W功率下提取20 min,N-亚硝胺的峰面积达到最大值,即提取效果最好。通过回收率试验选取活性炭固相萃取小柱为样品净化。UE-SPE-GC-NPD的回收率在66.80%~93.89%之间,其精密度在1.39%~3.07%之间。UE-SPE-HPLC-UV的回收率在65.80%~93.20%之间,其精密度均在1.19%~3.42%之间,该方法简便、快速,具有良好的灵敏度、重复性,适用于同时测定肉及肉糜制品中9种N-亚硝胺类化合物的含量。     

气相色谱-质谱法测定肉制品中的9种挥发性N-亚硝胺类物质

研究建立一种适用于肉制品中9种挥发性N-亚硝胺含量的气质联用快速检测方法。实验优化提取溶剂和色谱柱对提取和分离检测影响的条件,同时考察4种固相萃取单柱(酸性氧化铝、C18、活性炭、PSA)和1种双填料的混合固相萃取柱(PSA-C18)的净化效果。结果表明:本检测方法的线性系数均可达到0.999 2以上;线性范围为0~10μg/m L;重现性良好,相对标准方差均≤3.2%;回收率为85%~98%;检测限分别为N-亚硝基二甲基胺1.0μg/kg、N-亚硝基甲基乙基胺2.1μg/kg、N-亚硝基二丁基胺0.8μg/kg;其他均为0.5μg/kg。该方法能够满足测定肉及肉制品中N-亚硝胺的残留含量的需要。     

氢氧化钡处理-二氯甲烷萃取/GC-MS/MS检测几种水产品和加工肉制品中的7种N-亚硝胺

建立了氢氧化钡处理结合二氯甲烷萃取进行样品处理,气相色谱-串联质谱法检测几种水产品和加工肉制品中7种N-亚硝胺的新方法。以N-亚硝基二甲胺-d6、N-亚硝基二正丙胺-d14和N-亚硝基吡咯烷-d8为内标,10 g样品于50 mL离心管中经氢氧化钡溶液一步处理,离心后上清液再经二氯甲烷一次萃取,旋蒸浓缩至5 mL,氮吹至1 mL,DB-WAXUI柱(30 m×250 μm×0. 25 μm)进行色谱分离,多反应监测(MRM)模式进行质谱检测。该方法样品处理简便易行,7种N-亚硝胺在1~100 ng/mL浓度范围内线性良好(R2 > 0. 999);检出限为0.08~0.23 μg/kg,定量限为0.25~0.76 μg/kg;添加回收率为71.6%~133.8%,RSD为2.04%~17.1%。对市售9个鱼虾和8个加工肉制品的实际检测显示,N-亚硝基二甲胺的含量均在安全范围内。     

气相色谱-质谱法测定肉制品中的亚硝胺

利用二氯甲烷提取肉制品中的3种挥发性亚硝胺,即:N-二甲基亚硝胺(NDMA)、N-二乙基亚硝胺(NDEA)、N-二丙基亚硝胺(NDPA)。利用气质联用仪采用选择离子法(SIM)进行定性定量检测。本检测方法前处理简单快捷,易于操作,线性相关系数分别可达0.9991、0.9991、0.9995;线性范围分别可达0~250μg/mL;方法重现性良好,其RSD可达1.44%~1.99%;回收率可达90%~105%;灵敏度高,检测限分别为0.04μg/kg、0.025μg/kg、0.01μg/kg。     

气相色谱-质谱联用法测定肉制品中的4种N-亚硝胺类

本文建立了气相色谱质谱(GC-MS)快速测定肉制品中4种N-亚硝胺含量的分析方法,4种亚硝胺分别为N-二甲基亚硝胺(NDMA)、N-二乙基亚硝胺(NDEA)、N-二丙基亚硝胺(NDPA)、N-二甲基吡咯烷(NPYR)。样品经二氯甲烷提取后经固相萃取柱(SPE)净化,采用DB-1701柱分离,选择离子法(SIM)进行定性定量检测,4种亚硝胺在0.05~10μg/m L质量浓度范围内线性关系良好,相关系数均可达0.995以上,检出限0.06~0.1μg/kg,方法回收率75%~80%,标准偏差小于10%,此方法适用于肉制品中4种亚硝胺的测定。     

如皋火腿中挥发性N-亚硝胺种类和含量分析

用带有氮磷检测器的气相色谱(GC-NPD)测定了从市场上买来的20条如皋火腿中的挥发性N-亚硝胺,并用GC-MS确证GC-NPD检测结果.结果表明:市售如皋火腿中含有3种挥发性N-亚硝胺,分别为N-二甲基亚硝胺(NDMA)、N-二乙基亚硝胺(NDEA)和N-吡咯烷亚硝铵(NPYR), 平均含量分别为0.20、0.81和3.85μg/kg,其中NPYR的含量最多;NPYR的检出率最高为100%,其次为NDEA,检出率为95%, NDMA最小为85%,NDHA,NPIP和NDBA未检测出.     

氢氧化钡处理-分散液液微萃取结合气相色谱-串联质谱法测定肉制品中9种N-亚硝胺

目的 建立氢氧化钡碱溶液-分散液液微萃取结合气相色谱-串联质谱法(gaschromatography-tandem massspectrometry,GC-MS/MS)同时测定肉制品中9种N-亚硝胺类化合物的分析方法。方法 肉制品样品在80℃水浴中经氢氧化钡碱溶液皂化,去除油脂干扰,进一步将N-亚硝胺提取到水溶液中,再加入甲醇(分散剂)和二氯甲烷(萃取剂)进行高效萃取富集,在多反应监测模式下分析,稳定同位素内标法定量。对影响萃取效率的因素进行考察,如样品提取步骤中的皂化条件,无机盐、萃取剂和分散剂的种类及体积等。通过优化色谱、质谱参数和前处理条件,获得最佳检测结果。结果 除了N-亚硝基二甲胺(N-nitrosodimethylamine, NDMA)的线性范围为2.5～50.0 ng,其他8种N-亚硝胺类化合物在1.0～50.0 ng范围内线性关系良好, 9种N-亚硝胺类化合物的相关系数(r2)范围为0.9954～0.9999,方法检出限和定量限分别为0.1～0.2μg/kg和0.2～0.5μg/kg。在火腿、五香鸡肉和牛肉样品中分别进行0.5、5.0μg/kg浓度水平的加标实验,所有...     

响应面法优化籼稻挥发性成分SPME萃取条件的研究

应用顶空固相微萃取(SPME)技术结合气相-质谱法(GC-MS)对籼稻挥发性成分进行分析,并优化SPME的萃取条件。首先考察萃取量、萃取温度、平衡时间、萃取时间、解析时间对籼稻挥发性成分萃取的影响,在单因素试验的基础上进行响应面分析优化SPME萃取条件,以优化的最佳条件结合GC-MS对籼稻挥发性成分进行分析。结果表明:籼稻挥发性成分的最佳SPME萃取条件为萃取温度75℃、平衡时间59min、萃取时间60 min、解析时间5 min。籼稻含有烃类、醛类、含氮含氯含氧及杂环类、酸酯类、酮类、醇类等84种挥发性成分。     

固相微萃取结合气相色谱-质谱检测饮用水中 5种异味化合物

目的建立固相微萃取(SPME)结合气相色谱-质谱法检测饮用水中5种挥发性痕量异味化合物的分析方法。方法采用CAR/DVB/PDMS纤维涂层萃取头插入装有5种标准化合物的40 m L顶空瓶中,加入6 g Na Cl,80℃下平衡20 min,吸附40 min,经过气相色谱-质谱检测,对饮用水中常见的5种致异味化合物(2-甲基异莰醇(MIB)、2,4,6-三氯茴香醚(2,4,6-TCA),土臭素(GSM),2-甲氧基-3-异丙基吡嗪(IPMP),2-甲氧基-3-异丁基吡嗪(IBMP))进行检测。分别优化固相微萃取的萃取头、加盐量、萃取温度以及萃取时间等因素。结果最优提取条件:65μm PDMS/CAR/DVB纤维头,30%(m/v)加盐量,萃取温度60℃,萃取时间40 min。5种异味化合物在1~100 ng/L范围内线性关系良好,R20.971,检出限分别为1.0、1.0、0.8、1.0、1.0 ng/L,精密度小于10%。结论本方法检测限低,灵敏度高,是检测饮用水样异味的良好方法。     

酶法水解麦胚制取持水剂的研究

采用响应面分析方法研究了酶法水解麦胚制取持水剂的生产工艺，并对产品应用于香肠中的抗氧化效果进行了试验。试验结果表明：酶法水解麦胚制取持水剂的优化工艺参数为：对１０％的麦胚乳４００ｍｌ，反应温度为４４．４℃，反应时间为４ｈ，酶与底物浓度比为８６０μ／ｇ。经优化工艺生产的持水剂的水分活度为０．８９６，所对应的水解度为２６．５％。应用于香肠可显著提高其货架寿命。     

Effect of treatment with non-alcoholic beverages of patients with gastritis and hyposecretion

A positive effect of use of non-alcoholic drink "Shirinskaia high-vitaminized treatment-board Water" in complex treatment of chronic gastritis with hyposecretion was revealed.     

遮盖山羊绒“亮丝”的媒介/活性染色工艺

针对变异山羊绒的"亮丝"现象,以及不同染料在羊绒纤维不同位置上染的差异性,采用酸性媒介染料和毛用活性染料复配染色。结果表明,与单一染料染色工艺相比,复配染色技术通过对关键染料和助剂的精准控制,优化染色工艺,覆盖"亮丝"的效果良好。染色产品和染色废液中的铬含量均符合相关标准。     

Decontamination of broilers with hydrogen peroxide stabilised with glycerol during processing

Experiments were conducted to assess the effects of different concentrations of hydrogen peroxide stabilised by glycerol solution in potable water on the bacteriological and organoleptic quality of freshly slaughtered broiler carcasses. Skin-pH and colour were measured 3.5 and 24 h after treatment and compared to untreated carcasses. Bacterial colonisation was determined 3.5 and 24 h and, 7 days after treatment, carcasses being stored at 1 degrees C. None of the concentrations used affected the appearance and "bloom" of the carcasses as could be measured by colorimeter and changing of the acidity. Mean microbial counts were significantly reduced (P<0.01) when treated and control broilers were compared. Average reductions of 0.3 up to1.4 log N for the mesophilic aerobic counts were achieved and from 0.4 up to 1.2 log N for Enterobacteriaceae. A 3% w/w solution made from a commercially available stock solution (Glyroxyl), which consists of 44% hydrogen peroxide, 44% demineralised water and 12% glycerol proved to lower colonisation more effectively than a 2% solution.     

Relationship of Physicochemical Characteristics with Sensory Profile of Cookies Enriched with Medicinal Herbs

In this work, a range of model cookies enriched with different quantities of medicinal herbs, applied in two forms (pulverized mixture and extract), were studied to compare and describe relationships between physicochemical and sensory data. Multivariate statistical methods were applied to estimate relationships in the analyzed data. Analysis of variance showed that the majority of analyzed parameters were highly significant in discriminating among the samples (p < 0.05), which supported the usefulness of their application in characterizing the quality profile of enriched cookies. Principal component analysis on physicochemical data revealed that cookies at the same enrichment level showed more similarities. Principal component analysis on sensory data exhibited a larger separation between the samples with increasing enrichment levels, especially in the case of pulverized herbal mixture. According to partial least squares regression, two significant partial least squares components explained 92.7% and predicted 78.0% variation in the data. The most important parameters in discriminating between the cookies enriched with medicinal herbs were lightness, red tonality, and hardness. The selected physicochemical parameters could be used in future studies to evaluate variously enriched cookies by establishing models and investigating the predictability of sensory quality.     

酸解-酶膜联用法检测谷氨酰胺

研究了谷氨酰胺在酸性条件下的水解特性后 ,建立了酸解 酶膜联用的谷氨酰胺定量分析方法。此方法的线性范围为 10～ 40mmol/L ,相关系数R =0 .999,分析误差为 0 .1mmol/L ,测量所需时间约为 30min。     

猪皮制革必须适应市场经济

本文讨论了猪皮制革的现状,分析其成因,在此基础上阐明了猪皮制革必须适应市场经济的观点,并提出了猪皮制革走出低谷的若干具体对策。     

Synthesis of 2-Deoxy-maltooligosaccharides with Phosphorylase and Their Degradation with Amylases

By reaction of phosphorylase with D-glucal and inorganic phosphate instead of the natural substrate α-D-glucosyl phosphate novel 2-deoxy-maltooligosaccharides could be synthesized. Their properties and characterization by NMR spectroscopy, mass spectrometry and HPLC are described. Under similar conditions, except a higher phosphate concentration, 2-deoxy-α-D-glucosyl phosphate is obtained. This can also serve for the enzymatic elongation of the primer with 2-deoxy-glucosyl residues. The unnatural 2-deoxy-maltooligomers could be applied successfully as substrates for the exo-cleaving enzymes glucoamylase and β-amylase.     

强度为Weibul分布,应力为其他分布的可靠度求解

运用应力—强度相干理论,推导出强度为Ｗｅｉｂｕｌ分布,应力为其他分布时可靠度求解表达式,并应用专用数学软件Ｍａｔｈｅｍａｔｉｃａ实现了数值的求解。文中给出若干求解实例,求解的过程简便、直观,有利于工程可靠性设计与分析借鉴     

压力棒隔距块在纺细号纱上的应用

介绍了前区压力棒隔距块的结构和作用原理,探讨了压力棒隔距块在纺细号纱上的应用及工艺配置和技术要点;对比试验表明细纱前区加压力棒隔距块后,加强了对纤维的控制,有利于成纱质量的改善,尤其在细号纱上作用明显,但也要注意上车工艺一致性的调整,同时加强操作管理,否则会影响成纱条干的CVb值和纱疵数量.