快速气相色谱-质谱法分析非食用色素

气相色谱 -质谱法分析是一广泛使用的未知物分析方法[1 3 ] 。在 2 0 0 1年 6月全国性的食品打假工作中 ,岳阳市查处了数家食品加工厂和食品添加剂销售店 ,销售和使用一称为“金黄粉”的非食用色素。经快速气相色谱 -质谱法分析其挥发物成分 ,发现含有强致癌物二苯胺 ,从而证实该色素为非食用色素。该方法也可用于其他食品掺伪分析。1 仪器和试剂 :ＧＣ 1 7ＡＭＳ,ＣＬＡＳＳ 5 0 0 0(ＳＵＭＡＺＵ) ,毛细管气相色谱柱 :ＳＰＢＴＭ 1 (ｓｕｐｅｌｃｏＩｎｃ) ,柱号 :1 3 475 -0 3Ｂ ,柱子规格 :3 0ｍ× 0 3 2ｍｍ×0 2 5 μｍ。2 实验方…     

GC-MS联用分析测定志贺菌全细胞脂肪酸组成

目的：通过气相色谱-质谱法分析志贺菌全细胞脂肪酸，建立志贺菌全细胞脂肪酸的指纹图谱，为志贺菌的鉴定提供依据。方法：用气相色谱-质谱法分析了4种志贺菌的全细胞脂肪酸。结果：志贺菌全细胞脂肪酸主要脂肪酸有C12，C13，C14，C15，C16，C17，C18：1。志贺菌属脂肪酸成分都具有一定的特征，4个种之间也表现出一定的差异，标准菌株与地方菌株极其相似，同种不同来源的地方菌株表现出一定差异。结论：本结果为志贺菌的化学分类和快速鉴定提供参考资料。     

花生油脂肪酸特征模式的研究

目前国内外对食用油脂掺伪监测均采用传统的物理化学方法〔1,2〕。随着掺伪品种的多样化、复杂化 ,这些监测方法已难以作出准确判断 ,甚至出现误判。本文采用气相色谱 /质谱联用仪 (ＧＣ/ＭＳ)检测鉴别和确定花生油的脂肪酸组成 ,建立其特征脂肪酸组成模式 (ＦＡ模式 )并提出判断花生油掺杂的标准 ,应用本法可快速准确地判别出样品是纯正或掺杂。为食品卫生监督部门监测与控制食用油质量提供有效可行的依据。1　实验方法1 1　仪器和试剂　ＨＰ5 890ＧＣ/ 5 972ＭＳＤ气相色谱 /质谱联用仪 ;ＨＰ -ＩＮＮＯＷＡＸ弹性石英毛细管柱 2 5ｍ× 0 …     

超声萃取毛细管气相色谱法快速测定食品中环己基氨基磺酸钠

环己基氨基磺酸钠俗称甜蜜素，我国于1987年开始应用，是目前我国食品行业中应用最多的一种甜味剂。目前环己基氨基磺酸钠的检测方法主要有气相色谱法、液相色谱法、离子色谱法，另外有分光光度法和气相色谱-质谱法等方法，现有方法各有优缺点。我们应用超声萃取毛细管气相色谱法测定食品中环己基氨基磺酸钠，取得了满意的效果。     

气相色谱-质谱法测定血液中毒鼠强

本文研究了血液中毒鼠强的气相色谱—质谱法测定方法。血液通过有机溶剂直接萃取后，分离出毒鼠强，用气相色谱—质谱法进行定性、定量检测。25例中毒病人血液中毒鼠强浓度在0．0002-0．054μg／mL之间。     

GC-MS检测蔬菜有机磷农药残留的效果分析

目的:用比较法对气相色谱-质谱法检测蔬菜农药残留的效果进行综合分析。方法:用气相色谱-质谱法对已知的5种农药标准品连续稀释计算出检出限,并随机抽取本地菜农种植的四种蔬菜进行农药残留量检测。同时用气相色谱法同步进行比较试验。结果:两种方法比较,气相色谱-质谱法具有更高的灵敏度和准确度,差异有统计学意义(P<0.05)。对蔬菜残留农药的检测结果表明GC-MS在蔬菜农残检测中具有更广泛的用途。结论:GC-MS在检测蔬菜农药残留方面具有更好的效果。     

气相色谱-质谱法测定植物油中芥酸

目的　测定植物油中的芥酸。　方法　采用气相色谱分离 ,质谱定性 ,内标法定量。　结果　色谱峰分离好 ,无干扰。　结论　气相色谱 -质谱法测定植物油中芥酸快速准确 ,操作简便。     

气相色谱-质谱法同时检测七种氨基甲酸酯类杀虫剂

氨基甲酸酯类杀虫剂 (carbamateinsecticides)是继有机磷之后出现的一类农药 ,主要有呋喃丹、涕灭威、灭多威、残杀威、叶蝉散、速灭威、西维因等。具有杀虫效力强、作用迅速等特点。随着此类杀虫剂使用范围的不断扩大 ,由其引起的食物中毒、误服以及投毒事件时有发生。氨基甲酸酯类农药的测定方法主要有薄层层析法 ,气相色谱法 ,液相色谱法[1-2 ] ,液相色谱 -质谱法 ,气相色谱 -质谱法等[3 -4] ,但未见同时测定多种氨基甲酸酯的报道。气相色谱 -质谱法 (GC -MS)是近年来发展起来的大型仪器 ,其兼备气相色谱的高分离性能和质谱的高鉴别能…     

食物中农药残留分析方法的研究进展

本文综述了近年来农药残留分析的前处理技术和测定方法的研究进展，着重介绍了固相萃取法，凝胶渗透色谱法和超临界流体萃取法等前处理技术气相色谱－质谱法，液相色谱质谱法，超临界液体色谱等色谱测定方法以及毛细管电泳和生物技术在农药残留分析中的应用。     

国标中硫酸法不适合于油中掺加桐油的鉴别

目的　我们在使用国标方法中硫酸法鉴别食用植物油中的桐油时,发现此法用于芝麻油及含芝麻油的食用油和油中桐 油的鉴别时,往往出现假阳性。为此,对用硫酸法鉴别食用植物油中掺加桐油的检验方法的适用性进行了探讨。方法　国际 GB/T5009.37-2003的4.10油中桐油鉴别的4.10.1.3硫酸法。结果　发现使用硫酸法鉴别芝麻油及含芝麻油成分的食用 调和油时,无论其中含不含桐油均呈现棕红色,颜色越来越深,最后成为深棕黑色胶冻样粘状物,类似桐油阳性所显示的结 果。结论　硫酸法不适合于芝麻油及含芝麻油的食用调和油中桐油的定性鉴别。     

动植物油脂中反式脂肪酸测定方法的建立

目的建立适合国内条件的动植物油脂中反式脂肪酸测定方法,为国标方法提供依据。方法选择普通植物油、动物油和氢化植物油三个大类共9种动植物油脂样品,参照国际标准经部分修改,建立了适合国内条件的反式脂肪酸气相色谱分析及用面积归一法定量的测定方法,并进行了重复性测定和实验室间的验证。结果在实验条件下,油脂中脂肪酸可以得到很好的分离;除个别含量极低的脂肪酸外,各脂肪酸组分10次分析结果的相对标准偏差均小于10%,其中反式脂肪酸总和的RSD值在豆油和氢化豆油中分别是2.0%和0.3%;实验室间验证结果也表明,该方法在不同实验室间的结果有很好的一致性,豆油、氢化豆油、猪油三种样品的反式脂肪酸总和的RSD值分别是5.0%、1.1%和4.6%,均远小于10%。结论该检测方法实验室内和实验室间的精密度均较高,且所需仪器比较普及,操作步骤简单易行,分析时间短,适合国内开展,可作为我国动植物油脂反式脂肪酸的测定方法之一。     

A pilot study of open label sesame oil in hypertensive diabetics

The objective of this study was to investigate the effect of sesame oil in hypertensive diabetics medicated with atenolol (beta-blocker) and glibenclamide (sulfonylurea). This open label trial with two intervention periods comprised 22 male and 18 female patients, 45-65 years old, with mild to moderate hypertension and diabetes. Sesame oil (Idhayam Gingelly oil, V.V.V. & Sons, Virudhunagar, Tamilnadu, India) was supplied to the patients, who were instructed to use it in place of other cooking oils for 45 days. Blood pressure (BP), anthropometric measurements, plasma glucose, glycated hemoglobin (HbA1c), lipid profiles [total cholesterol, low-density lipoprotein cholesterol (LDL-C), and high-density lipoprotein cholesterol, and triglycerides (TG)], lipid peroxidation [thiobarbituric acid-reactive substances (TBARS)], electrolytes (sodium, potassium, and chloride), and enzymic (superoxide dismutase, glutathione peroxidase, and catalase) and nonenzymic (vitamin C, vitamin E, beta-carotene, and reduced glutathione) antioxidants were measured at baseline and after 45 days of sesame oil substitution. The same patients were then switched over to other oils like palm or groundnut oils as their regular oils at random for another 45 days, and the investigations were carried out again at the end. Systolic and diastolic BP decreased remarkably. When oil substitution was withdrawn, BP values rose again. Body weight, body mass index, girth of waist, girth of hip, and waist:hip ratio were reduced upon substitution of sesame oil. Plasma glucose, HbA1c, TC, LDL-C, and TG were decreased. TBARS level was reduced, while the activities of enzymic and the levels of nonenzymic antioxidants were increased. Plasma sodium levels were reduced, while potassium levels were elevated. These results indicate that substitution of sesame oil as the sole edible oil has an additive effect in further lowering BP and plasma glucose in hypertensive diabetics.     

Non-destructive discrimination of sesame oils via hyperspectral image analysis

Sesame oil is produced from cheap imported raw materials, but its quality differs depending on the imported form. The purpose of this study was to determine the quality characteristics of sesame oil through hyperspectral image (HSI) analysis. The following types of sesame oil samples were used in this study: sesame oil WS (WS1, WS2) prepared using imported whole-sesame seeds, sesame oil SP (SP1, SP2) prepared using only imported sesame powder and sesame oil WSP (WSP1, WSP2) prepared by mixing imported sesame powder with whole-sesame seeds. The principal component analysis revealed that WS and SP or WS and WSP had different principal components. As a result of partial least squares-discriminant analysis, WS and WSP had an average R² of 0.9289 in a training model, and prediction R² was the highest at 0.8333 in a test model. The developed model was affected by C-H stretch second overtones for fatty acids and C-H and O-H bonds corresponding to phenolic absorbance. The average R² of partial least squares regression developed owing to fatty acid and phenolic compound content was the highest. Therefore, it was possible to analyze the quality characteristics of sesame oil according to the form of raw material using hyperspectral image.     

Benzo(a)pyrene contamination of vegetable oils

Benzo(a)pyrene (B(a)P) analysis was carried out with glass chromatographic column with alumina followed by reverse phase high-performance liquid chromatography (HPLC) and spectrofluorometric detection. B(a)P level in 40 vegetable oils were as follow: from 0.11 to 0.38 microg/kg in olive; from 0.92 to 3.74 microg/kg in rape seed oils; from 0.11 to 2.25 microg/kg in sunflower oils and from 0.33 to 1.26 microg/kg in soya oils. In another investigated oils: arachide (peanut) corn, safflower, linen, hempen, sesame, pumpkin seeds, grape seeds---values from 0.10 to 1.44 microg/kg and 3.83 microg/kg in sea buckthorn oil were detected. B(a)P concentration in 4 from 40 investigated oils exceed the 2 ppb limit proposed by the European Commission. Heating of sample of oils: olive, rape, soya, linen, corn, sesame, peanut, in temp. 240 degrees C for 30 min. has not influence on decreased of B(a)P level.     

鱼油类保健品中不饱和脂肪酸的气相色谱及质谱检测研究

[目的 ]　研究鱼油中多不饱和脂肪酸含量的确证分析方法。　 [方法 ]　利用毛细管气相色谱以及气质联用技术检测鱼油中多不饱和脂肪酸 (如DHA、EPA、DPA)的含量。　 [结果 ]　建立了用毛细管色谱柱进行有效分离 ,保留时间定性 ,以面积归一法或外标法定量 ,以GC -MS法进行确证的有效方法 ,同时对标准质谱库 (NIST库 )中没有的成分 (如DPA、DHA)建立了标准谱图。　 [结论 ]　本方法能满足对鱼油产品中不饱和脂肪酸的分析要求 ,具有简便、快速、可靠的特点     

微波萃取技术在食用植物油与潲水油中胆固醇含量测定的应用

目的:建立植物油类物质(火锅油、潲水油、地沟油及食用植物油)中胆固醇含量测定前处理的快捷方法,并采用超高液相-串联四极杆质谱(UPLC-MS/MS)技术定量分析。方法:采用微波萃取技术对植物油类物质进行皂化处理,再用石油醚-乙醚(1∶1)提取后,以2,2,3,4,4,6-d6胆固醇为内标,采用UPLC-MS/MS法,大气压化学电离源(APCI)正离子模式,多反应检测方式测定胆固醇浓度。结果:与传统水浴加热皂化方法前处理植物油类物质比较,微波萃取皂化前处理方法简变、快捷、高效、低污染等优点,测得胆固醇的含量几乎无显著性差别,方法回收率为98%。结论:微波萃取皂化前处理方法可用于植物油类物质中胆固醇含量测定。     

High-performance liquid chromatographic determination of vitamin D3 in fish liver oils and eel body oils

Identification and determination of vitamin D3 (or D2) and 25-OH-D3 in fish liver oils and eel body oils were carried out. By co-chromatography on HPLC, UV spectra and/or GC-MS, vitamin D3 was identified in naturally occurring fish liver oils and eel body oils, whereas a drop of fish liver oil contained supplemented vitamin D2. 25-OH-D3 was identified only in skipjack liver oil. The HPLC method proposed in a previous report (Takeuchi, A. et al. (1984): J. Nutr. Sci. Vitaminol., 30, 11-25) was confirmed to also be useful for determination of vitamin D3 (or D2) in fish liver oils and eel body oils. The assayed values of vitamin D3 in skipjack and tuna liver oils were 57,760 and 16,200 IU/g, respectively, which were much higher than those in cod and pollack liver oils. The assayed values of vitamin D3 in eel body oils were very low (16-43 IU/g) and showed no appreciable change despite differences in the farming conditions. Determination of 25-OH-D3 in skipjack oil was performed by using HPLC, and the assayed value was 1.8 micrograms/g. This was about 1/800 lower than that of vitamin D3.     

Direct metabolic fingerprinting of olive oils using STELDI-MS

A new and rapid approach for analysis of olive oil has been developed using sorptive tape-like extraction in combination with laser desorption ionization mass spectrometry (STELDI-MS). This powerful combination has some great advantages, as no-separation steps, solvent-free, matrix-free, and no sample preparation. The olive oil compounds are analyzed by LDI-MS, directly from the sample spot in a thin-layer chromatography (TLC) plate. Chosen samples represent products commonly used as adulterants in extra virgin olive oil (EVOO) and the main monitored ions were lipid adulteration markers. Analytical procedures consisted of profiling the main fatty acids (m/z 255 – palmitic acid, 279 – linoleic acid, 281 – oleic acid and 283 – stearic acid), triacylglycerols (m/z 901 – LLL and 907 – OOO) and some phenolic compounds (m/z 169 – gallic acid, 193 – ferulic acid and 195 – 2(4-hydroxyphenyl) ethyl acetate) in extra virgin olive oil (EVOO), olive oil (OO), hazelnut oil (HO) and soybean oil (SO). Compound identification was confirmed by analysis of collision-induced dissociation (CID) products in positive (ion [M+Na]⁺) and negative mode (ion [M−H]⁻). This method is simple, fast and efficient in identifying compounds that can be used to recognize different levels of adulteration, oxidation and hydrolysis of vegetables oils.     

天津市1998年煎炸油的卫生状况调查及与10年前的对比分析

为了解当前煎炸油使用中的卫生状况及影响因素,为煎炸食品的卫生监督提供参考,依据当前煎炸食品生产方式,按个体、国营与合资３类,分层随机抽取２９、３８及３０例,共９７例煎炸点。进行现场卫生学调查、采样,采用国家标准方法对煎炸油样品的酸价（ＡＶ）、羰基值（ＣＯＶ）、极性组份（ＰＣ）等指标进行分析,并与１９８７年的结果进行比较。结果显示煎炸油的少变程度因所用煎炸原料油品种的不同而有差别,其中精炼的高烹油最     

Corn and sesame oils increase serum gamma-tocopherol concentrations in healthy Swedish women

We studied the effects of dietary intervention with three vegetable oils (Linola, corn or sesame oil, all good sources of gamma-tocopherol) on absolute and relative concentrations of alpha- and gamma-tocopherol in human serum. The oils contained only small amounts of linolenic acid but varying amounts of oleic and linoleic acids, and they had different concentrations of alpha-tocopherol. Forty healthy female students (mean age 26 y) were randomly assigned to one of three groups and consumed a diet that contained one of the three oils for 4 wk. Refined oils were distributed as ingredients in specially prepared buns, in margarine or as dressing. Serum tocopherols, serum lipoproteins and plasma malondialdehyde concentrations were measured. The gamma-tocopherol concentrations normalized to serum lipids increased significantly in the corn and sesame oil groups (P < 0.01), and the alpha-/gamma-tocopherol ratios decreased significantly from baseline concentrations in all groups (P < 0.05). The alpha-tocopherol concentrations did not change during the diet period in any of the three groups. Serum cholesterol, serum apolipoprotein B and plasma malondialdehyde concentrations decreased significantly only in the Linola oil group (P < 0.05). These data show that a moderately modified natural diet that contains both alpha- and gamma-tocopherol increases the serum gamma-tocopherol concentration in healthy women without affecting the serum alpha-tocopherol concentration.