超高效液相色谱-串联质谱法快速测定火锅底料中的5种罂粟壳生物碱残留

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法检测火锅底料中吗啡、可待因、那可丁、罂粟碱、蒂巴因5种生物碱残留的分析方法。样品经含0.2%甲酸的乙腈提取,PRi ME HLB固相萃取小柱快速净化,ACQUITY BHE C18色谱柱(1.7μm,2.1 mm×50 mm)分离,以p H 8.0氨水溶液和乙腈作为流动相,梯度洗脱,经电喷雾正离子(ESI+)模式电离及多反应监测(MRM)测定目标化合物,采用基质标准溶液曲线法定量分析。结果表明,吗啡、可待因的线性范围为0.25~100μg/L,蒂巴因的线性范围为0.05~100μg/L,那可丁、罂粟碱的线性范围为0.05~10μg/L,相关系数均大于0.999。5种生物碱的检出限为0.9~4.5μg/kg,定量下限为3.0~15.0μg/kg;在1、5、10μg/kg(吗啡和可待因为5、25、50μg/kg)3个加标水平下的回收率为70.7%~109.6%,相对标准偏差小于11%。该方法操作快速简单、灵敏度高,适用于火锅底料中罂粟壳生物碱残留的定性与定量分析。     

微波消解-电感耦合等离子体质谱法测定养生保健汤料包中16种稀土元素

采用电感耦合等离子体质谱法测定养生保健汤料包中16种稀土元素。采用硝酸-过氧化氢混合液为消化剂对样品进行微波消解,利用电感耦合等离子体质谱法测定16种稀土元素。16种稀土元素的质量浓度在1.0~80μg·L-1范围内呈线性,检出限(3S/N)为0.1~1.7μg·kg-1。方法用于标准物质的分析,测定值与认定值相符。按方法分析样品做精密度试验,测定值的相对标准偏差(n=10)小于5%。方法用于测定12种养生保健汤料中稀土氧化物含量总和在0.127~0.984 mg·kg-1之间。     

Effect of long-term heat exposure on rheological and intrinsic water characteristics of bone-derived beef stocks

Bone-derived protein stocks are used in food industry to enhance taste of soups, sauces, and a range of other products. Both during commercial manufacturing and when used for culinary purposes, the stocks may be exposed to high temperatures for an extended time period. The present study investigated the effect of retention at 90°C for 0, 3, 6, 9, 24, 48, 72, and 168 hr on the functional attributes of concentrated bone-derived beef stocks (57% Dry matter (DM)). Visual inspection and rheological analyses showed that during increasing heat exposure, the gel strength as well as viscosity of the concentrated stocks decreased incrementally and significantly (P > 0.001). Nuclear magnetic resonance (NMR) relaxation measurements conducted on the beef stocks also revealed strong effects of heat exposure on the transverse (T₂) relaxation time, which increased incrementally and significantly (P > 0.001) with longer heat exposure. Thus, the present study demonstrated that heat-induced changes in rheological properties of bone-derived beef stocks can be ascribed to changes in intrinsic water–protein interactions and water attributes as a result of heat-induced protein modifications. In conclusion, the study proves that NMR relaxometry is a valuable tool for monitoring changes in intrinsic water mobility that are manifested in modified functional attributes of concentrated beef stocks.     

Comparison of Different Volatile Extraction Methods for the Identification of Fishy Off-Odor in Fish By-Products

This study was conducted to analyze volatile odor compounds and key odor-active compounds in the fish soup using fish scarp and bone. Five extraction methods, including solid-phase microextraction (SPME), dynamic headspace sampling (DHS), solvent-assisted flavor evaporation (SAFE), stir bar sorptive extraction (SBSE), liquid-liquid extraction (LLE), were compared and SPME was finally selected as the best extraction method for further study. The volatile odor compounds were analyzed by gas chromatography-olfactometry-mass spectrometry (GC-O-MS) and comprehensive two-dimensional gas chromatography-olfactometry-mass spectrometry (GC × GC-O-MS) techniques, and the key odor-active compounds were identified via aroma extract dilution analysis (AEDA) and relative odor activity value (r-OAV) calculation. A total of 38 volatile compounds were identified by GC-O-MS, among which 10 were declared as odor-active compounds. Whereas 39 volatile compounds were identified by GC × GC-O-MS, among which 12 were declared as odor-active compounds. The study results revealed that 1-octen-3-one, 2-pentylfuran, (E)-2-octenal, 1-octen-3-one, hexanal, 1-octen-3-ol, 6-methylhept-5-en-2-one, (E,Z)-2,6-nondienal and 2-ethyl-3,5-dimethylpyrazine were the key odor-active compounds in the fish soup.     

浙江古城墙传统灰浆材料的分析研究

灰浆材料一直是古代建筑类文化遗产研究的重要对象,文保工程中使用传统灰浆的诸多优点已广为人知,在认识传统灰浆的基础上开发新的石灰基粘结保护材料已然成为国际研究热点。随着中国的经济发展,很多古建筑的保护也开始提上日程,然而关于中国传统灰浆材料的研究颇为薄弱。实地调查浙江地区多座古代城墙遗址,采集灰浆样品,利用多功能密度仪、粉末X射线衍射仪(XRD)、傅里叶红外光谱仪(FTIR)、热重-差热分析仪(TG-DSC)和湿化学分析技术,对浙江地区7处古城墙灰浆样品进行了分析检测和研究。结果表明：这些古城墙使用的胶结材料是纯“白灰灰浆”,主要成分是碳酸钙,含量在75%～90%之间,其原料主要是钙质生石灰,个别来自镁质生石灰;其中有4座城墙灰浆添加有糯米成分,说明该地区在明代向灰浆里添加糯米等有机材料是建筑城墙十分普遍的工艺技术;检测发现这些建筑灰浆的密度较低,且数值相差较大,在1.2～1.9 g·cm-3之间,应是环境长期侵蚀的结果。同时,也分析了这些砌筑灰浆的其他物化特征,为下一步古城墙本体保护和保护材料的研发,以及传统灰浆全国范围内的比较研究提供了科学依据。     

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结合HL-2A 装置的参数,在电子回旋共振加热(ECRH)离(在)轴加热的情况下,研究高能量捕获电子驱动的鱼骨模不稳定性。数值结果表明,高能量电子极向比压βh 大于某一个比压阈值βh,crit 时,鱼骨模会被高能量电子激发,其频率随高能量电子极向比压的增大而缓慢增加且与高能量电子的环向进动频率一致;比压阈值βh,crit 随着高能量电子密度剖面峰化程度的增加而减小,但当密度剖面增大到一定值时比压阈值βh,crit 趋近于一个常数。此外,还分析了箍缩角和扰动能对鱼骨模实频和增长率的影响。发现在箍缩角α0 =1附近增长率有一极小值,表明高能量勉强通行电子对鱼骨模具有稳定作用;而扰动能 δWˆc增大时,鱼骨模表现出实频变大而增长率变小的特征,这表明了本底等离子体对鱼骨模有一定的稳定效果。     

Flavor mechanism of micro-nanoparticles and correlation analysis between flavor substances in thermoultrasonic treated fishbone soup

To study the physicochemical properties of micro-nanoparticles (MNPs) in thermoultrasonic treated fishbone soup, it was subjected to ultra-filtration with a 100 kDa ultrafiltration membrane to obtain large MNPs (LMNPs) and small MNPs (SMNPs). LMNPs and SMNPs were treated with force-breakers, and the interactions of the MNPs with five characteristic volatile compounds were investigated. LMNPs covered most proteins (222.66 mg/mL) and fatty acids (363.76 mg/g), while SMNPs was mostly soluble small molecules with taste substances like total free amino acids (85.26 mg/g), organic acids (2.55 mg/mL), and 5′-nucleotides (169.17 mg/100 mL). The stability of LMNPs is significantly higher than raw bone soup, and SMNPs can exist stably in the solution. Correlation analysis between flavor substance content and flavor suggested that the overall flavor profile of halibut bone soup was closely related to the content changes of 72 significant influence variables. The binding of LMNPs to characteristic flavor compounds was largely affected by hydrophobic interactions, hydrogen bonds, and ionic effects. While the binding of SMNPs to characteristic flavor compounds was largely determined by hydrophobic interaction and hydrogen bonding. This study explores the characteristics of MNPs and provides the possibility to clarify the interaction mechanism between MNPs and flavor.