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建立了用氨基固相萃取小柱净化提取液,液相色谱串联质谱(LC-MS/MS)法测定食用油中辣椒素和二氢辣椒素含量的检测方法。结果表明,辣椒素在0~100 ng/mL范围内线性关系良好(R2 = 0.998 6),平均回收率在70.6%~90.5%,相对标准偏差(RSD,n=3)在3.1%~8.9%,检出限为0.03 μg/kg;二氢辣椒素在0~20 ng/mL范围内线性关系良好(R2 = 0.998 8),平均回收率在71.5%~100.7%,相对标准偏差(RSD,n=3)在6.0%~13.2%,检出限为0.006 μg/kg。该方法简便快速、准确可靠,是鉴别地沟油和测定食用油中辣椒素类物质的有效方法。 相似文献
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近年来,植物油掺伪问题频发,现有理化特性和感官特性检测已无法满足相关的检测需求。由于检测时间长、检测成本高,以及复杂的检测过程导致气相色谱法和高效液相色谱法等仪器分析方法的应用受限。近期,新型传感技术、新材料和数字信息技术、电子鼻技术、机器视觉技术、组学技术等的发展为快速准确鉴别植物油掺伪提供了技术支持。有鉴于此,以食用植物油掺伪研究为对象,综述了近期国内外对植物油掺伪检测的重要研究进展,讨论了光谱检测技术、色谱检测技术、电子鼻检测技术、机器视觉技术、组学技术等分析方法的特点以及发展现状,并对植物油掺伪鉴别技术的发展进行了展望,以期为植物油的掺伪检测提供一定的理论参考。 相似文献
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目的:提高食用油脂质量鉴定结果的准确性。方法:建立食用油脂中合成辣椒素、天然辣椒素和二氢辣椒素含量不确定度的数学模型,对检测过程中可能引入不确定度的因素进行分析,并对各不确定度分量进行评定。结果:食用油脂中合成辣椒素、天然辣椒素和二氢辣椒素含量分别为(0.250±0.032),(0.123±0.015),(0.130±0.014) μg/kg,k=2。结论:该不确定度主要来源于标准曲线的线性拟合和液相色谱质谱联用仪的分析引入的不确定度。 相似文献
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《Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment》2013,30(4):660-665
Cyromazine and dicyclanil are both used as insect growth regulators. This paper describes an easy and innovative simultaneous extraction method for residues of cyromazine and dicyclanil in food of animal origin, and a confirmation procedure using UHPLC-MS/MS. The sample was extracted, deproteinised by 1% trichloracetic acid in water-acetonitrile, followed by selective defatting using hexane based on the degree of matrix complexity; cleaned-up on an mixed-mode cation exchange (MCX) cartridge; and quantified by using matrix-matched calibration. The mean recoveries were all between 62.0% and 99.2%, and the RSDs were all below 9.94%. The present method was rapid, sensitive and reliable, which was applied to the quantitative analysis of these residues in animal tissues. 相似文献
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食用植物油与餐厨废油脂中三酰甘油氧化聚合物含量的研究 总被引:2,自引:0,他引:2
为了探寻餐厨废油脂的标志性氧化产物,采用正相硅胶柱制备色谱预分离油脂中极性物,联用高效体积排阻色谱方法测定三酰甘油氧化聚合物(oxidized triacylglycerol polymers,TGP),统计分析了12种常见品种44个新鲜食用植物油样品和具代表性的三大类61个来源不同、精炼程度各异的餐厨废油脂样品的TGP含量,显示食用植物油中TGP平均质量分数为(0.68±0.37)%,精炼餐厨废油脂中平均质量分数为(6.10±3.44)%,二者TGP含量具极显著差异(P<0.01)。结果表明TGP可望成为鉴别源于餐厨废弃食用油的二次油的指标。 相似文献
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以加标植物油为研究对象,通过优化前处理条件,用有机溶剂一步萃取植物油中的辣椒素和二氢辣椒素,再结合高效液相色谱和荧光检测器,建立了一种植物油中辣椒素、二氢辣椒素的快速检测方法。优化的前处理条件为:甲醇为萃取溶剂,萃取溶剂体积30 mL(油样质量30 g),萃取次数2次,每次萃取时间10 min。优化条件下,辣椒素、二氢辣椒素的回收率为81.08%~100.28%,日内、日间相对标准偏差分别在0.18%~1.92%和0.55%~5.14%范围内,两种目标物的检出限均为5 μg/kg。该方法前处理较为简单,省时省力、检测成本较低、实用性强,为植物油中辣椒素、二氢辣椒素提供了一种新的检测方法。 相似文献
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对超高效液相色谱-串联质谱测定猪肉中甲氧氯普胺残留量过程中可能影响到结果准确性的因素进行了分析。根据行业标准SN/T 2227-2008《进出口动物源性食品中甲氧氯普胺残留量检测方法液相色谱法-质谱/质谱法》,建立不确定度评价的数学模型,通过不确定度来源分析建立不确定度的评价方法。结果表明:标准溶液浓度产生的不确定最大,随机效应引入的不确定度次之,样品定容产生的不确定度最小。猪肉中甲氧氯普胺残留量为50.1μg/kg时,其扩展不确定度为5.0μg/kg(k=2)。 相似文献
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《Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment》2013,30(7):1201-1210
ABSTRACTThe detection of mycotoxin contamination in foodstuffs is highly significant for public health. Herein we report an analytical method based on magnetic solid-phase extraction (MSPE) and UPLC-MS/MS for the simultaneous determination of mycotoxins, including fumonisins B1 (FB1), zearalenone (ZON) and ochratoxin A (OTA), in vegetable oil. Magnetic nanoparticles coated with double layers of silicon dioxide were synthesised and found to be an effective MSPE adsorbent for mycotoxins. The proposed MSPE procedure serves not only for sample clean-up but also for mycotoxin enrichment that enhances greatly the assay’s sensitivity. Under the selected MSPE conditions, linear matrix-matched calibration curves were obtained for mycotoxins in a concentration range from 0.178 to 625 μg kg–1. The limits of detection were 0.210 μg kg–1 for FB1, 0.0800 μg kg–1 for OTA and 1.03 μg kg–1 for ZON. The proposed MSPE UPLC-MS/MS method was applied for the determination of mycotoxins in vegetable oil samples, including maize oil, rapeseed oil and soybean oil. ZON was detected in a maize oil at 101 μg kg–1, which is below the European Union limit of 200 μg kg–1 in foodstuffs. 相似文献
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建立了一种高分辨质谱(Triple-TOF-MS/MS)测定芝麻油、葵花籽油、大豆油、菜籽油、花生油和玉米油等常见食用植物油中甘油三酯的方法,分析并确定不同食用植物油中每种碳原子当量(ECN)下的甘油三酯组成与含量。结果表明:采用Triple-TOF-MS/MS法可以根据一级质谱母离子(加氢母离子、加钠离子和加氨母离子)相对分子质量以及二级质谱的碎片离子([DAG]~+)对相同ECN的甘油三酯进行定性分析。采用该方法对芝麻油、葵花籽油、大豆油、菜籽油、花生油和玉米油进行甘油三酯检测,结果共获得35种甘油三酯,均含有LnLL、LLL、LLO、PLL、LOO、PLO和OOO 7种甘油三酯。 相似文献
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液相色谱-串联质谱法检测食用油脂中多环芳烃 总被引:4,自引:3,他引:4
建立了有机溶剂萃取、硅胶固相萃取柱净化、液相色谱-串联质谱法(LC-MS/MS法)测定食用油脂中EPA 16种多环芳烃的检测方法。EPA 16种多环芳烃的定量限分别为0.02~0.43μg/kg,回收率为86.5%~104.6%,日内精密度小于6%,日间精密度小于5%。在40个受测油脂样品中,EPA 16种多环芳烃的含量范围为11.68~146.06μg/kg。对照我国GB 2716规定,所有受测样品中苯并(a)芘含量均不超过≤10μg/kg的限量标准。然而,8个油样的苯并(a)芘含量超过了欧盟≤2μg/kg的限量标准,10个油样的PAH4含量超过了欧盟≤10μg/kg的限量标准。 相似文献
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目的 建立一种超高效液相色谱-串联质谱测定食用油脂中辣椒素的分析方法。方法 试样经正己烷溶解,氢氧化钠水溶液提取,碱性提取液经硫酸酸化后,过PEP-2固相萃取小柱净化,采用超高效液相色谱-串联质谱仪检测,外标法定量。以ACQUITY UPLC BEH C18色谱柱(3.0mm×100mm,1.7μm)为固定相,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源正离子模式和多反应监测模式。结果 天然辣椒素、二氢辣椒素、合成辣椒素的质量浓度在0.1μg/L~100μg/L内与其对应的峰面积呈线性关系,检出限(3S/N)合成辣椒素为0.01 μg/kg;天然辣椒素为0.006 μg/kg;二氢辣椒素为0.005 μg/kg。以空白样品为基体进行加标回收试验,回收率在80.3%~96.2%,测定值的相对标准偏差(n=6)为4.5%~5.6%。结论 该方法快速、准确,能满足食用油脂中辣椒素的快速筛查和检测要求。 相似文献
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Tran T Thanh Marie‐France Vergnes Jacques Kaloustian Tarek F El‐Moselhy Marie‐Jo Amiot‐Carlin Henri Portugal 《Journal of the science of food and agriculture》2006,86(2):220-225
Phytosterols can be of value in decreasing cardiovascular risk of coronary heart disease. β‐Sitosterol was the most abundant sterol in the three oils studied (sunflower, olive and ‘4 oil mixture’). The total phytosterol level was the highest in the ‘4 oil mixture’ compared with the other oils studied. Tests performed on the effect of aging (heating at 50 °C for several weeks and at 100 °C for 1 h) did not show any significant variation in the phytosterol content. In contrast, heating at 200 °C for 1 h led to a 50–60% decrease of phytosterol in the oils studied and in the standard solutions. Copyright © 2005 Society of Chemical Industry 相似文献
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目的采用气相色谱-质谱(GC-MS)对大豆油、芝麻油、花生油、橄榄油、葡萄籽油5种食用植物油中挥发性成分进行分析。方法采用顶空固相微萃取(HS-SPME)技术对5种食用植物油中的挥发性成分进行萃取,并结合气相色谱-质谱(GC-MS)技术对挥发性成分进行测定。结果 5种食用植物油中共检测出101种挥发性化合物,其中大豆油11种、花生油28种、芝麻油65种、橄榄油25种、葡萄籽油5种。主要包括醛类、酯类、醇类、杂环类、酚类、酸类等10类物质。大豆油中主要的挥发性成分有戊醛、已醛和己酸,花生油中主要的挥发性成分有己醛、2,5-二甲基吡嗪和2,3-二氢苯并呋喃;芝麻油中主要的挥发性成分为5-甲基呋喃醛、2-吡咯甲醛、糠醇、愈创木酚、2-甲基吡嗪、2-乙基-6甲基吡嗪等;橄榄油中主要的挥发性成分为叶醇和4-己烯-1-醇乙酸酯;葡萄籽油中主要的挥发性成分为已醛。结论 5种食用植物油的挥发性物质的种类和含量上有很大区别,可为食用植物油的掺假鉴别提供参考依据。 相似文献
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采用超高效液相色谱串联三重四极杆质谱(UPLC-MS/MS)法测定绿茶、红茶和乌龙茶中丙烯酰胺含量。样品2.0 g经正己烷去脂和乙腈提取,MCX固相萃取柱净化,采用Waters BEH-C18色谱柱分离,以0.1%的甲酸水溶液和乙腈溶液为流动相进行梯度洗脱;质谱条件采用电喷雾离子源(ESI)和多反应监测模式(MRM),同位素内标法定量。结果表明,丙烯酰胺的质量浓度为5.0~160.0 μg/L时,线性关系良好,相关系数(R2)>0.999,且精密度实验结果的相对标准偏差(RSD)为1.73%,定量限为1.5 μg/kg,加标回收率为88.0%~96.8%。说明该方法精密度及准确度良好,能满足茶叶中丙烯酰胺含量检测的要求。 相似文献
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Virgin olive oil was mixed with eight vegetable oils (sunflower, soya bean, palm, linseed, cottonseed, corn, sesame, and olive residue) at various levels. The Bellier test was applied to find the minimum detectable adulteration level and the ‘sensitivity score’ for each oil. The test was inapplicable to sunflower and linseed oils regardless of the level in olive oil. It was successful in detecting olive residue, soya bean, palm, cottonseed, corn, and sesame oils at minimal levels of 730, 150, 130, 90, 60 and 10 g kg?1, respectively. The rancidity level of the adulterant oils did not affect the performance of the test in the case of sunflower, linseed and sesame oils. The sensitivity of the test decreased considerably with increasing peroxide value of the adulterant oil: soya bean, palm, cottonseed, corn and olive residue. However, the change in sensitivity level commenced at so high a peroxide value that it has no significance for practical purposes; at such levels of peroxidation the adulterated olive would be unmarketable and rejected by inspectors due to its poor sensory quality. 相似文献
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目的:建立植物油中黄曲霉毒素B1含量的液相质谱-串联质谱测定方法。方法:采用液相色谱-串联质谱法(LC-MS/MS),以乙腈为溶剂提取植物油中黄曲霉毒素B1。ZORBAX SB-C18(2.1mm×50mm,1.8μm)色谱柱,流动相为乙腈-0.2%甲酸(40∶60)梯度洗脱,流速为0.3mL/min,进样量为5μL。采用电喷雾离子化四极杆串联质谱,多反应监测方式测定样品的浓度。检测离子对分别为m/z 313.0→285.0和m/z 313.0→241.0。结果:黄曲霉毒素B1进样量在0.2044.08ng/mL(r=0.9991)范围内呈良好的线性关系,平均加样回收率为98.15%,RSD=1.12%(n=9)。结论:该法简便快捷、结果准确,可用于植物油中黄曲霉毒素B1的含量的测定。 相似文献