Chemometric deconvolution of gas chromatographic unresolved conjugated linoleic acid isomers triplet in milk samples

A generally known problem of GC separation of trans-7;cis-9; cis-9,trans-11; and trans-8,cis-10 CLA (conjugated linoleic acid) isomers was studied by GC–MS on 100 m capillary column coated with cyanopropyl silicone phase at isothermal column temperatures in a range of 140–170 °C. The resolution of these CLA isomers obtained at given conditions was not high enough for direct quantitative analysis, but it was, however, sufficient for the determination of their peak areas by commercial deconvolution software. Resolution factors of overlapped CLA isomers determined by the separation of a model CLA mixture prepared by mixing of a commercial CLA mixture and CLA isomer fraction obtained by the HPLC semi-preparative separation of milk fatty acids methyl esters were used to validate the deconvolution procedure. Developed deconvolution procedure allowed the determination of the content of studied CLA isomers in ewes’ and cows’ milk samples, where dominant isomer cis-9,trans-11 is eluted between two small isomers trans-7,cis-9 and trans-8,cis-10 (in the ratio up to 1:100).     

HPLC-ELSD与GC-MS法测定牛乳甘油三酯sn-2位脂肪酸组成

研究建立了快速、准确测定牛乳脂肪甘油三酯sn-2位脂肪酸组成的方法．利用胰脂酶专一水解甘油三酯sn-1和sn-3位置上的脂肪酸得到sn-2单甘油酯和游离脂肪酸,再通过蒸发光散射高效液相色谱分离出sn-2位单甘油酯,然后对其进行衍生,用气相色谱质谱联用仪对sn-2脂肪酸组成进行分析．结果显示用蒸发光散射高效液相色谱法分离sn-2位单甘油酯时方法的回收率达到83．3％～85．1％,该法省去了传统测定中费时费力的薄层色谱分离步骤．用气相色谱质谱联用法对产物进行分析,精密度高,结果可靠．分析结果表明,牛乳脂肪sn-2位脂肪酸由2．57％月桂酸、7．68％豆蔻酸、34．74％棕榈酸、11．56％亚油酸、22．53％油酸和15．21％硬酯酸组成．     

高效液相色谱法测定动物组织中3-甲基喹喔啉-2-羧酸残留量

本文建立了猪、鸡、鱼肌肉及猪、鸡肝脏组织中喹乙醇代谢残留标识物3-甲基喹喔啉-2-羧酸残留量的高效液相色谱分析方法.样品在酸性环境水解,经乙酸乙酯、磷酸盐缓冲溶液依次提取,Oasis MAX固相萃取柱净化,高效液相色谱紫外测定(HPLC-UV).3-甲基喹喔啉-2-羧酸标准曲线相关系数(r2)为0.9992(10～1 000 μg/L);不同动物组织样品中3-甲基喹喔啉-2-羧酸工作曲线相关系数(r)为0.9995～0.9997(2～100 μg/kg).在2～100 μg/kg浓度范围,3-甲基喹喔啉-2-羧酸回收率为69%～104%,日内相对标准偏差＜15%,日间相对标准偏差＜20%.检出限(CCα)为1.2～4.3 μg/kg,定量限(CCβ)为2.0～5.6 μg/kg.     

拉曼光谱法测定天然脂肪球脂质成分

天然脂肪球主要由甘油三酯构成,以不同大小的球状形式分泌而得。不同大小的脂肪球的球体和膜组成成分不同,从而影响了脂肪在乳中的存在形式和最终的乳品功能特性。然而,不同大小的脂肪球成分的差异尚未完全阐明。利用拉曼光谱测定特定大小脂肪球及膜的脂质和脂肪酸组成。拉曼光谱能够从单个脂肪球获得特定拉曼信号,并且在不破坏天然脂肪球构型的情况下进行测定。结果显示,小脂肪球在2 885/2 850 cm-1处条带信号较高,表明小脂肪球趋于形成结晶态的脂肪球膜包裹流动态的甘油三酯内核的结构。此外,小脂肪球与大脂肪球相比,1 655/1 443 cm-1的条带信号较低,表明小脂肪球的脂肪酸不饱和程度较高。总之,从本实验结果可以推断,用特定的小脂肪球分离而得的稀奶油在熔化时较大脂肪球难熔化,搅拌耗时更多,但能形成更柔软的黄油。     

THM-Py-GC/MS分析内蒙古伊和淖尔出土照明燃料

考古发掘出土的遗物中,有机残留物大部分是以附着在器物上,或者是遗址表面而存在的,由于没有固定形状,或量少而难以发现,且不易保存,因此常常被忽视。但是这类有机物作为古代人类生活生产资料,包含重要的历史信息,具有珍贵价值。通过遗址中发现的器物或者有机残留物,可以决定器物甚至是遗址的用途,古代照明燃料就属于这类有机残留物。中国古代多使用动物油、植物油、蜡等作为照明燃料,对植物油和蜡都有一定研究,但对于动物油种类的分析仅停留在区分反刍动物与非反刍动物。引入热裂解气相色谱质谱技术（THM-Py-GC/MS）研究有机残留物,使用600 ℃裂解温度经过12 s裂解时间,可以将甘油三酯与老化过程中由于失去酰基逐步形成的双酰基甘油、单酰基甘油等完全裂解成甘油与脂肪酸,通过计算脂肪酸相对含量,可以分析不同动物油具有的特征。同时用高温裂解代替了传统酸化提纯样品的预处理方法,能最大程度的保留样品中的各组分。加入过量的四甲基氢氧化铵,可将样品中脂肪酸与醇等量转化为对应的酯和醚,在气相色谱初始50 ℃保持5 min,然后以10 ℃·min-1升至280 ℃保持10 min的条件下,将甲基化的样品组分分离,质谱以1∶100的分流比进行测定。对内蒙古伊和淖尔墓地出土铁灯内的残留物进行了分析,结果显示,灯内残留物样品中主要成分是C7-C22连续碳原子的脂肪酸,含量较高的饱和脂肪酸有十四烷酸、十五烷酸、十六烷酸、十七烷酸、十八烷酸等。对比老化前与老化后猪油、牛油、羊油等动物脂肪参考样品所含主要成分与相对含量,老化后的羊油中的奇数碳饱和脂肪酸含量明显高于其他两种动物油,并且这一特征也体现在考古样品中,结合以往文献中动物油成分的研究结果,可以判断出残留物中所含动物油的确切种类属羊油。此外样品中包含的碳氢化合物与醇属于蜡的成分,根据脂肪酸及醇的相对含量可以判断为蜂蜡。热裂解气相色谱质谱技术（THM-Py-GC/MS）,为出土有机残留物,特别是动物脂肪种类的的分析研究,提供了更加高效、便捷的方法。并且,对混合有机残留物种类的鉴别也做出了有益的尝试。     

A new complex plant for carbonization and composting of municipal wastes

A new complex plant for carbonization and composting of municipal wastes proposed for Gero City is introduced. The separated combustible waste and non-separated combustible waste are carbonized in two fluidized carbonization furnaces in the plant, and the coke produced is used in steelworks. The separated garbage and forest-wastes are mixed with dried septic-tank sludge to produce high quality compost for farms. This use of waste materials in the complex plant considerably lowers the amount of waste going to land-fills, and in addition, creates lower total emission of dioxins and carbon dioxide into the environment.     

Extraction and Stabilization of Betalains from Beetroot (Beta vulgaris) Wastes Using Deep Eutectic Solvents

Deep eutectic solvents (DES) using magnesium chloride hexahydrate [MgCl₂·6H₂O] and urea [U] proportions (1:1) and (2:1), were prepared for their use as extracting and stabilizer agents for red and violet betalains from beetroot (Beta vulgaris) waste. The synthetized DES [MgCl₂·6H₂O] [U] showed similar properties to eutectic mixtures, such as, liquid phase, low melting points and conductivity, thermal stability, and variable viscosity. In turn, betalain DES extracts (2:1) exhibited compatibility in the extraction and recovery of betalains from beetroot wastes, showing a betalain content comparable to that of betalain extracts. Betalain stability was determined by degradation tests; the exposure conditions were visible light (12 h), molecular oxygen from atmospheric air and environmental temperature (20–27 °C) for 40 days. The kinetic curves of the betalain degradation of water samples depicted a first-order model, indicating the alteration of a violet colouration of betalains from beetroot waste for 5–7 days. However, betalains from DES extracts were kept under visible light for 150 days, and for 340 days in storage (amber vessels), achieving a stability of 75% in comparison with initial beet extracts.     

牛奶的保鲜

本文介绍了牛奶的保鲜方法,说明了牛奶致腐的原因,概述了因微生物的作用所导致的牛奶中乳糖、蛋白质和脂肪3种主要成分的变化,并简单介绍了这些变化的反应机理。     

On-Site Measurement of Fat and Protein Contents in Milk Using Mobile NMR Technology

Robust and easy-to-use NMR sensor technology is proposed for accurate, on-site determination of fat and protein contents in milk. The two parameters are determined using fast consecutive ¹H and ³⁵Cl low-field NMR experiments on milk samples upon the 1:1 addition of a low-cost contrast solution. Reliable and accurate measurements are obtained without tedious calibrations and the need for extensive database information and may readily be conducted by non-experts in production site environments. This enables on-site application at farms or dairies, or use in laboratories harvesting significant reductions in costs and time per analysis as compared to wet-chemistry analysis. The performance is demonstrated for calibration samples, various supermarket milk products, and raw milk samples, of which some were analyzed directly in the milking room. To illustrate the wide application range, the supermarket milk products included both conventionally/organically produced, lactose-free milk, cow’s, sheep’s and goat’s milk, homogenized and unhomogenized milk, and a broad nutrient range (0.1–9% fat, 1–6% protein). Excellent agreement between NMR measurements and reference values, without corrections or changes in calibration for various products and during extensive periods of experiment conduction (4 months) demonstrates the robustness of the procedure and instrumentation. For the raw milk samples, correlations between NMR and IR, NMR and wet-chemistry, as well as IR and wet-chemistry results, show that NMR, in terms of accuracy, compares favorably with the other methods.     

HPLC-APCI(+)MS/MS分析动物源性食品中的硝基咪唑类药物残留量

运用高效液相色谱-大气压电离串联四极杆质谱(HPLC-APCI( )MS/MS)内标法分析动物源性食品中多种硝基咪唑类(nitroimidazoles)药物——甲硝唑(MNZ)、地美硝唑(DMZ)、替硝唑(TNZ)、洛硝唑(RNZ)的含量。样品添加氘代标示物HMMNI-D3、IPZ-OH-D3后,用乙腈提取,通过OASIS HLB C18SPE柱净化,Waters Sunfire C18色谱柱分离,采用梯度洗脱,流动相为0.1%甲酸水溶液和0.1%甲酸乙腈溶液;大气压电离源正离子MRM模式检测:MNZm/z172.0/82.1,172.0/128.0;DMZm/z142.0/81.1,142.0/96.1;TNZm/z248.0/121.0,248.0/93.1;RNZm/z201.0/140.0,201.0/110.0;IPZ-OH-D3m/z189.0/125.0,189.0/171.0;HMMNI-D3m/z161.0/58.0,161.0/143.1。方法定量下限(LOQ,S/N>10)0.2μg/kg,在质量浓度0.2~25.0μg/L范围内,峰面积与质量浓度成良好线性(r>0.999 1)。