Untargeted fatty acid profiles based on the selected ion monitoring mode

Fatty acids are potential biomarkers of some diseases and also key markers and quality parameters of different dietary fats and related products. Thus, untargeted fatty acid profiles are important in the study of dietary fat quality and fat-related diseases, as well as in other fields such as bioenergy. In addition, accurate identification of unknown components is a technological breakthrough for the selected ion monitoring (SIM) mode for untargeted profiles. In this study, we developed untargeted fatty acid profiles based on SIM. We also investigated mass spectral characteristics and equivalent chain lengths (ECL) to eliminate the influence of non-FAMEs for identifying fatty acids in samples. As an application example, fatty acid profiles were used to classify three edible vegetable oils. The results indicated that SIM-based untargeted fatty acid profiles could yield accurate qualitative and quantitative results for more fatty acids and benefit related studies of metabolite profiles.     

固相萃取-气相色谱-串联质谱法测定大葱等蔬菜中23种邻苯二甲酸酯类化合物残留

建立了气相色谱-串联质谱联用(GC-MS/MS)同时测定蔬菜中23种邻苯二甲酸酯类化合物(塑化剂)的方法。蔬菜经乙腈提取,玻璃Florisil固相萃取柱净化,正己烷定容,Agilent DB-5MS UI超高惰性毛细管柱(30 m×0.25 mm×0.25 μm)程序升温分离,MS/MS(选择反应监测模式)分析,外标法定量。考察了大葱等复杂基质蔬菜中邻苯二甲酸酯类化合物的提取和净化方法,并对色谱和质谱条件进行了优化,提出了扣除本底的办法;通过基质加标校准曲线补偿对邻苯二甲酸酯检测的基质效应。23种邻苯二甲酸酯的线性范围除邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)为0.1~5 mg/L外,其余均为0.02~1 mg/L,相关系数(r)除邻苯二甲酸二(2-甲氧基乙基)酯(DMEP)外均大于0.99。方法的检出限(S/N=3)为0.01~0.05 mg/kg,定量限(S/N=10)为0.02~0.1 mg/kg。3个加标水平下目标物的平均回收率为81.3%~104.2%,相对标准偏差(n=6)为3.2%~11.2%。该方法稳定可靠,应用串联质谱很好地消除了基质效应的干扰,灵敏度高,定性定量更为准确,适用于蔬菜中邻苯二甲酸酯类化合物的检测和确证。     

液相色谱-串联质谱法快速筛查测定浓缩果蔬汁中的156种农药残留

建立了浓缩果蔬汁中156种农药多残留的液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)测定方法。样品用1%醋酸乙腈溶液萃取,经Waters Sep-Pak Vac固相萃取柱净化,乙腈-甲苯(体积比为3∶1)洗脱,旋转蒸发浓缩,用乙腈-水（体积比为3∶2）溶解,以Agilent ZORBAX SB-C18色谱柱分离,以电喷雾电离串联质谱在正离子多反应监测(MRM)模式下进行测定。对156种农药在5种浓缩果蔬汁(橙汁、苹果汁、葡萄汁、白菜汁、胡萝卜汁)中两个添加水平下的回收率进行了测定,回收率范围为57.2%～122.7%,相对标准偏差范围为0.9%～19.8%。方法的检出限(S/N=3)和定量限(S/N=10)范围分别为0.10～56.77 μg/kg和0.33～189.23 μg/kg。该方法样品前处理简单、快速、分析时间短,灵敏度、准确度和精密度均符合农药多残留检测技术的要求,适用于苹果汁、橙汁、葡萄汁、白菜汁、胡萝卜汁等浓缩果蔬汁中156种农药多残留的快速筛查测定。     

高效液相色谱法测定蔬菜中利佛米及其主要代谢物的残留量

用甲醇提取试样中的利佛米及其代谢产物[4－氯,-a,a,a-三氯代-N－（1-氨-2-丙氧基亚乙基）－O-甲苯胺],用二氯甲烷反提取,蒸干二氯甲烷层,其残留物用流动相溶解,供配有紫外检测器的高效液相色谱仪测定,外标法定量。分别测定利佛米和其主要代谢物后再计算以利佛米计的总残留量。     

植物油荧光光谱有效信息提取及其自动分类

植物油市场中出售的芝麻油、玉米油和花生油有多种品牌,不同品牌间价格差距较大,且存在假冒的现象,利用荧光光谱技术可以无损地鉴别购买油种是否为标签所标种类。主成分分析方法及平行因子方法可对这3种油种进行人工分类,但其存在类间距离相比于类内距离过小的不足,在结合传统的聚类分析方法时,会造成误分类现象。本文以提高类间距离、达到正确聚类为目标,经过比较分析,选择均值、标准差、光谱重心坐标、二阶混合中心距、相关系数、等价椭圆二倍倾角正切值、在重心激发波长处的发射光谱的偏度系数和峰度系数作为统计参数,相比于直接使用聚类方法,芝麻油分类的正确率从92.3%提高到100%,玉米油分类的正确率从75%提高到100%,花生油从57.1%提高到100%。用偏最小二乘判别分析方法验证了本文方法的合理性。本文方法可以用于植物油检测仪器的自动分类,利于市场监管及指导人们日常消费。     

A convenient ultrasound‐assisted saponification for the simultaneous determination of vitamin E isomers in vegetable oil by HPLC with fluorescence detection

An efficient ultrasound‐assisted saponification was developed for simultaneous determination of vitamin E isomers in vegetable oil by high‐performance liquid chromatography with fluorescence detection. The samples were saponified ultrasonically with potassium hydroxide solution for only 7 min, then the analytes were extracted with ether. Vitamin E isomers were separated on a C₁₈ column at 25°C with a mobile phase of methanol/acetonitrile (81:19, v/v) at a flow rate of 0.8 mL/min. Fluorescence detection was operated at 290 nm of excitation wavelength and 327 nm of emission wavelength. Under the optimized conditions, good linearities over the range of 0.001–8.00 μg/mL (r > 0.999) were obtained. Mean recoveries of the method were 88.0–106%, with intra‐ and interday RSDs less than 11.8 and 12.8%, respectively. The detection limits and quantification limits of the method were 0.30–1.8 and 1.0–6.1 μg/kg, respectively. The recoveries of this method were much higher than that of the quick, easy, cheap, effective, rugged, and safe method and direct dilution method, but were similar to those of hot saponification. This proposed method provides reliable, simple, and rapid quantification of vitamin E isomers in vegetable oils. Five kinds of vegetable oils were analyzed, the quantification results were within the ranges reported by other authors.     

Tetraphenylethene Functionalized Polyhedral Oligomeric Silsesquioxane Fluorescent Probe for Rapid and Selective Trifluralin Sensing in Vegetables and Fruits

A novel fluorescent probe was designed and synthesized from tetraphenylethene (TPE) and polyhedral oligomeric silsesquioxanes (POSS) via Heck-palladium catalyzed cross-coupling reaction. The as-synthesized TPE functionalized probe performed good solvent stability and selectively preconcentration capability towards target analyte due to its stable structure and the adsorption property. The morphology as well as the physical and chemical properties of the POSS@TPE were carefully characterized. The POSS@TPE was employed to develop an effective fluorescent probe for trifluralin, with a response range of 0.1-80 mg/kg and a detection limit of 0.102 mg/kg. The mixed mechanisms of inner-filter effect (IFE) and photoinduced electron transfer (PET) explain the selectivity of POSS@TPE. Rapid detection for trifluralin in tomato and celery has been achieved with recoveries between 99.4–120.7% (RSD≤3.4%), and the results were verified compared with GC-MS method.     

Lubricants from renewable energy sources – a review

Lubricant oils are known to decrease the friction coefficient between two contacting surfaces. It is essential for the correct function of almost the totality of mechanical machinery working in the entire world. Lubricant oils consist of about 80% of oily base stocks which attributes to their properties of viscosity, stability, and pour point to the lubricant plus additives supplemented to improve these properties. Petroleum lubricants are usually environmentally unacceptable due to their low biodegradability and toxicity. These oils contaminate the air, soil, and drinking water and affect human and plant life to a great extent. Thus, the demand for environmentally acceptable lubricants is increasing along with the public concerns for a pollution-free environment. Plant oils are promising as base fluid for biolubricants because of their excellent lubricity, biodegradability, viscosity–temperature characteristics, and low volatility. The purpose of this paper is to present a survey of the current status of biolubricating oil. This research provides an overview on the synthesis, tribochemical behavior; the effect of structure on friction/wear, load-bearing capacity, resistance to rise in specimen temperature, and varying response of antiwear/extreme-pressure additives in the presence of vegetable oil/derivative structures has also been discussed. Though a significant number of papers have been published in this area, there is still much to explore. A proper selection of base oil and additives is therefore essential for an efficient synthesis of biolubricating oil.     

分光光度法测定新鲜蔬菜中维生素C的含量

水溶性的维生素C是一种人体必需的营养物质。维生素C是含有烯二醇基的多羟基内酯结构,利用其水溶液在波长265nm处有较强烈的紫外吸收峰,建立了直接用紫外分光光度法测定新鲜蔬菜中维生素C含量的方法。实验结果表明,维生素C的含量在1.0~12.0μg/mL内线性关系良好,线性方程为A=0.066 03c+0.019 74(R2=0.997 51),检出限为0.044μg/mL,样品加标回收率为97.5%~105.4%。方法操作简单,准确度高,对新鲜蔬菜的测定结果令人满意。