气相色谱质谱联用法测定不同塑料包装植物油中邻苯二甲酸酯类

建立了气相色谱质谱联用法测定不同塑料包装植物油中邻苯二甲酸酯类的检测方法。对不同塑料包装植物油采取不同的分离和净化方法,优化了凝胶渗透色谱分离条件。结果表明:该方法对邻苯二甲酸酯类的最低检测限为0.01~0.05 mg/kg,相关系数为0.9965~0.9990,加标回收率为83.1%~98.6%,RSD为1.94%~4.73%。应用本方法分析了食用植物油中邻苯二甲酯类物质含量,经与标准GB/T 21911方法相比,表明该方法操作简单、测定结果准确,可以作为植物油中邻苯二甲酸酯类化合物的确证方法。      

自动顶空-气相色谱-串联质谱法测定生乳中8种苯系物的研究

建立生乳中8种苯系物同时测定的自动顶空-气相色谱-串联质谱法。 方法 试样中的苯系物经顶空进样器加热挥发后进入HP-InnoWax（30m*0.25mm,0.25μm）毛细管色谱柱进行分离,气相色谱质谱联用仪进行测定,外标法定量。 结果 8种苯系物在0-25.6ng/mL浓度范围内线性良好,相关系数大于0.99,,定量限为0.1-0.8μg/kg、回收率为85.0%～106.8%、精密度均小于7%。 结论 本方法前处理简单、灵敏度高,可以满足生乳中8种苯系物的同时测定要求。     

Survey of furan in heat processed foods by headspace gas chromatography/mass spectrometry and estimated adult exposure

Furan is a suspected human carcinogen that is formed in some processed foods at low ng per g levels. Recent improvements in analytical methodology and scientific instrumentation have made it possible to accurately measure the amount of furan in a wide variety of foods. Results from analysis of more than 300 processed foods are presented. Furan was found at levels ranging from non-detectable (LOD, 0.2-0.9 ng g^-1) to over 100 ng g^-1. Exposure estimates for several adult food types were calculated, with brewed coffee being the major source of furan in the adult diet (0.15 µg kg^-1 body weight day^-1). Estimates of mean exposure to furan for different subpopulations were calculated. For consumers 2 years and older, the intake is estimated to be about 0.2 µg kg^-1 body weight day^-1.     

Survey of furan in heat processed foods by headspace gas chromatography/mass spectrometry and estimated adult exposure

Furan is a suspected human carcinogen that is formed in some processed foods at low ng per g levels. Recent improvements in analytical methodology and scientific instrumentation have made it possible to accurately measure the amount of furan in a wide variety of foods. Results from analysis of more than 300 processed foods are presented. Furan was found at levels ranging from non-detectable (LOD, 0.2–0.9 ng g^?1) to over 100 ng g^?1. Exposure estimates for several adult food types were calculated, with brewed coffee being the major source of furan in the adult diet (0.15 µg kg^?1 body weight day^?1). Estimates of mean exposure to furan for different subpopulations were calculated. For consumers 2 years and older, the intake is estimated to be about 0.2 µg kg^?1 body weight day^?1.     

Determination of molecular and free sulphur dioxide in foods by headspace gas chromatography

A study was made of the equilibria between SO2 in packaged liquid foods and gaseous SO2 in their headspace atmospheres as a basis for a new analytical method for the determination of molecular and free SO,. Using a gas-chromatographic method developed previously to determine SO2 at the 1 × 10⁻³ mg/l level in atmospheres saturated with water vapour, studies with aqueous solutions showed that headspace SO2 was directly proportional to molecular SOz in accordance with Henry's law.
Using the Henry's law constant for the S02/H20 system, determinations of molecular SOz were made on a white and a red wine and a fruit juice, each adjusted to five levels of pH to achieve different concentrations of molecular SO,. The results observed by the headspace method showed good agreement with those determined by a reference analytical method with white wine and fruit juice, but with red wine the reference method gave values which were more than 45% higher. Free SO2 was determined in a range of white wines by the headspace and reference methods, and the results showed high correlations.
The headspace method is rapid, precise and non-destructive. A major advantage is that, during the analysis, it does not change the complicated equilibria between SO, and its ionised species, hence complexes of SO2 and food constituents are not disturbed.     

顶空气相色谱法测定卷烟包装材料中的溶剂残留

采用顶空气相色谱法对卷烟包装材料中残留溶剂(乙酸乙酯、乙酸丁酯、甲苯、乙苯等)进行分析,并讨论了各种条件对测定的影响。分析结果表明,该方法对4种残留溶剂的线性范围分别为乙酸乙酯0.4~120 mg/L,甲苯0.4~120 mg/L,乙酸丁酯1.2~600mg/L,乙苯0.5~150 mg/L,测定结果的相对标准偏差为2.6%~3.1%,样品的回收率为90%~95%;方法简便、快速、重现性好,该方法可用于一些卷烟包装材料中溶剂残留的分析。      

卷烟包装纸中挥发性有机化合物(VOCs)的顶空-气相色谱分析

采用顶空-气相色谱法分析了卷烟包装纸中的16种挥发性有机化合物(VOCs),方法快速简便,准确可靠。对部分国内卷烟包装纸进行了检测,并对卷烟包装纸的VOCs现状进行了讨论。      

Static headspace gas chromatography of acetaldehyde in aqueous foods and polythene terephthalate

Polythene terephthalate (PET) is frequently used as a packaging material for mineral water and other non-alcoholic beverages. PET contains detectable amounts of acetaldehyde, which is able to migrate to its packed product. An automated headspace gas Chromatographic method for the determination of acetaldehyde has been developed and was used for the quantification of acetaldehyde in aqueous food products and their PET packages. A cold trap, mounted in the GC oven, between the autosampler and analytical column was introduced as a new application. The detection limit of acetaldehyde was found to be 3 ng/ml with a standard deviation of 3%. The contents of acetaldehyde found in carbonated mineral water and lemonades ranged between 11 ng/ml and 7447 ng/ml, while the contents of acetaldehyde in the PET packages ranged from 1.1 g/g to 3.8 g/g.     

Distillation-extraction of styrene migrating from polystyrene containers to foods by gas chromatography

A simple, accurate and sensitive gas-liquid chromatographic method has been developed for the determination of styrene migrating from polystyrene containers into foodstuffs. an apparatus for the extraction of styrene was designed for the purpose, based on the BP apparatus for the determination of volatile oils. Styrene was extracted from foods by distillation with concurrent extraction from the distillate by n -hexane. Extraction was complete in 35 min. Hexane extracts were analysed by GC-FID using a glass column with durene as internal standard. Styrene levels in containers were from 1.7 to 192 μg g⁻¹ and in foods from 0.013 to 0.13 μg g⁻¹.     

Determination of acrylamide monomer in hydroponically grown tomato fruits by capillary gas chromatography—mass spectrometry

Tomato (Lycopersicon esculentum L) fruits from plants grown hydroponically on polyacrylamide gel were obtained in order to assess any possible uptake of acrylamide monomer from the nutrient solution to the fruit during cultivation. Analysis of acrylamide in the gel itself involved aqueous extraction, bromination and then capillary GC determination with nitrogen-specific detection. By standard addition a level of 0·18 ± 0·01 g kg^?1 residual monomer was found to be present in a sample of gel used by an experimental horticultural station. Tomato fruits were analysed by extraction of the aqueous phase, bromination, silica-gel cartridge clean-up and capillary GC–MS determination by selected ion monitoring. The recovery of the method was 26–62% but losses throughout were compensated for by use of 2,3-dibromo-2-dimethylpropionamide internal standard. No acrylamide monomer could be detected in tomato fruits from plants grown hydroponically on polyacrylamide gel at a limit of detection of 1 × 10^?6 g kg^?1, demonstrating that the monomer is not transferred from the growing medium into tomato fruits.     

Determination of acrylonitrile monomer in food packaging materials and in foods

An automated headspace gas chromatographic method is described using nitrogen specific detection for the quantification of acrylonitrile monomer (AN) in acrylonitrile-butadiene-styrene (ABS) food packaging tubs and in the contained foods. For a limited number of retail foods, levels of AN in ABS tubs (ranging from 2 to 10 mg/kg) and their contents (soft margarine, butter and shortening) are reported (ranging from 0.01 to 0.05 mg/kg), the results being confirmed by mass spectrometry (low and medium resolution selected ion monitoring). The latter technique was also used to quantify the levels of AN in the coatings of retail packaging films on a range of substrates, which were found to be between <0.001 and 0.02 mg/m².     

顶空气相色谱法测定白酒中氰化物含量

目的建立顶空气相色谱法测定白酒中氰化物含量检测的方法,探究GB5009.36-2016第二法在白酒、白兰地、威士忌、朗姆酒等酒样中应用的区别。方法将酒样进碱解前处理后,以顶空进样器注入气相色谱仪进行分离,电子捕获检测器进行检测。以加标回收率为指标,对方法及前处理进行评价。结果国标第一法与第二法结果有较大的差别,碱解前处理的气相色谱法与国标第一法结果相近。用GB 5009.36-2016第二法测定白酒、白兰地、威士忌、朗姆酒等中的氰化物含量时,均无法得到较好的加标回收率;用GB5009.36-2016第二法检测伏特加、以食用酒精为酒基的露酒中的氰化物含量时可以得到较好的回收率。顶空气相色谱法测定白酒中氰化物含量时,线性相关系数r为0.9999,相对标准偏差(relative standard deviation,RSD)为8.0%,回收率为78.0%～1112.5%。结论顶空气相色谱法测定白酒中氰化物含量时能够得到与国标第一法相近的结果,该方法操简单、灵敏度高,结果准确度高,适合白酒中氰化物含量的测定。     

Quantitative analysis of styrene monomer in foods. A limited East Australian Survey

The levels of styrene monomer in foods packaged in polystyrene containers were determined by a headspace gas chromatography (g.c.) method and two reversed phase high-performance liquid chromatography (h.p.l.c.) methods. A total of 146 samples were analysed from Victoria and New South Wales which included yoghurt, cream, cheese, dessert, ice cream, egg white, onion dip and margarine. The highest level of styrene found was 0.1 mg kg^?1 in yoghurt. About 85% of all yoghurt samples were found to have values less than 0.05 mg kg^?1. The lowest values of styrene obtained were for margarine samples, of which more than 90% contained less than 0.010 mg kg^?1. The estimated limits of detection of the h.p.l.c. methods for all products except margarine were 0.005 mg kg^?1. The h.p.l.c. detection limit for margarine and the g.c. method for yoghurt were estimated to be 0.01 mg kg^?1.     

顶空固相微萃取-气相色谱-质谱法测定大曲中的土臭素

土臭素（geosmin,GSM）是引起白酒土霉味的一种主要化合物,是在大曲制造过程中由微生物产生的。本文建立了一种简便、快速的顶空固相微萃取气相色谱质谱法（HS-SPME-GC-MS）测定大曲中GSM。大曲样品采用乙醇水溶液进行提取,蒸馏后经HS-SPME处理,GC-MS进行分析,外标法定量。在100⁸000ng/kg的质量浓度范围内,GSM有较好的线性关系,相关系数（r）大于0.99。通过对大曲空白样品进行加标回收率实验和精密度实验考察方法的可行性。结果表明GSM的回收率为89.19%⁹8.49%,相对标准偏差介于2.15%与3.06%之间。GSM的检出限为42.6ng/kg,定量限为140.6ng/kg。本方法适用于大曲中GSM的检测。      

气相色谱-质谱法测定食品用纸制品中五氯酚含量

目的 建立气相色谱-质谱法测定食品用纸制品中五氯酚含量的分析方法,了解食品用纸制品中五氯酚的残留状况.方法 纸制品试样加入2,4,6-三溴酚内标后,经液-液萃取,SLC柱净化,乙酸酐-吡啶溶液衍生后,采用气相色谱-质谱法测定,内标法定量.结果 在50～1000 ng范围内,相关系数均>0.9995.方法 的检出限为0....     

An accurate quantitative method for the analysis of terpenes in milk fat by headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry

HS-SPME analysis of terpenes does usually have inherent quantification problems when working with complex samples, especially due to the matrix effect of the substrate or the calibration solution. Three different terpene carrier matrices were compared: methanol, synthetic oil and milk fat obtained by centrifugation from milk cream. Considerable differences in calibration sensitivity parameters were observed depending on the matrix used and on the type of terpene standard analysed. For milk sample quantification purposes internal standard method was preferred using milk fat as calibration matrix. Linearity range, repeatability, recovery and limits of detection and quantification were determined. Validation parameters were different depending on the concentration and molecular structure of each terpene analysed, particularly between mono- and sesquiterpenes. The method was useful to determine in an accurate manner the terpene content in milk samples from pasture fed animals, and it will help to establish objective terpene levels to differentiate milks from specific production systems.     

毛细管气相色谱法测定聚氯乙烯食品包装中的氯乙烯单体

研究采用毛细管气相色谱法检测聚氯乙烯薄膜中残留的氯乙烯单体,并用气相色谱质谱法进行确证.样品中的氯乙烯单体采用静态顶空技术提取.利用极性毛细管气相色谱柱进行分离并结合氢火焰离子化检测器进行高灵敏度检测.氟乙烯单体在0.05～0.2 mg/L的浓度范围内有较好的线性关系,相关系数为0.999,相对标准偏差在3.1%以内,检测低限为0.5 mg/kg,该方法具有较好的检测精密度和灵敏度.     

全自动固相萃取-气相色谱-三重四级杆质谱法检测蔬菜中23种农药残留

目的建立蔬菜中有机磷类、拟除虫菊酯类共23种农药残留的分析方法。方法样品加丙酮-二氯甲烷(1∶1,V/V)混合溶剂提取后经全自动固相萃取仪净化,采用气相色谱-三重四级杆串联质谱的多反应监测模式进行检测,内标法定量。结果 23种农药在0.05~0.80 mg/L范围内线性良好,相关系数均大于0.993 3;加标回收率在75.0%~105.5%之间;方法的检出限为0.02~0.70 mg/kg。在少量蔬菜样品中发现氯氰菊酯和氯氟氰菊酯超标。结论该方法适用于蔬菜中多种农药残留的快速筛查测定。