食品风味物质前处理及分析方法研究进展

食品风味对消费、生产和科学研究至关重要。然而,食品风味化合物通常在产品中的浓度较低,构成成分相对复杂,这给它们的提取、分离和定量带来了挑战。快速、灵敏、准确的样品制备方法对测定食品中微量风味化合物起着至关重要的作用。样品制备的方法繁多,本文重点讨论了固相萃取、固相微萃取、搅拌棒吸附萃取、溶剂辅助风味蒸发、静态顶空、动态顶空、液-液萃取、同时蒸馏萃取的原理特点及应用。并对常用的色谱质谱和电子鼻技术进行了介绍。其中气相色谱-质谱联用法、气相色谱-离子迁移谱联用法、气相色谱-嗅觉-质谱联用法、全二维气相色谱-飞行时间质谱联用法是常用的色谱质谱方法。本文综述了食品风味物质的前处理和检测分析方法,以期为食品行业提供参考和借鉴。     

烟草特有亚硝胺分析研究进展

综述了近年来烟草及卷烟烟气中亚硝胺的分析方法:气相色谱-热能检测器法、气相色谱-质谱联用法、液相色谱质-质谱联用法、液相色谱质-质谱-质谱联用法等.指出,建立分析速度快、定量准确、重现性好、分析成本低的烟草特有亚硝胺分析法将是今后该领域研究的方向.     

气相色谱-串联质谱在食品农药残留检测中的应用进展

正气相色谱-质谱联用(GC-MS)综合气相色谱和质谱两种检测方法的特点,既具有气相色谱法分离能力较强的特点,又具有质谱检测法对化合物的结构准确鉴定的特点,能同时准确且快速地检测食品中微量的多种农药残留及其衍生物质。因此,在各国家食品检测中得到较为广泛的应用,笔者根据实际工作经验从各个层面分析现阶段我国食品农药残留检测中使用到的气相色谱-质谱联用法,并以此     

气质联用法测定柑橘类水果12种农药残留

<正>随着我国化工业的逐渐发展,农作物的药物生长作用成为我国农业辅助发展的主要手段。在这样的背景下,我国农作物的农药残留比率逐渐增加,严重影响人们的生命健康和安全。因此,从农药残留检验的角度出发对其研究具有重要的研究价值和意义。气质联用法及其原理气质联用法气质联用法指将气相色谱和质谱相结合的一种测量方式,其秉承气相色谱的分离能力、质谱的化合物灵敏度测量能力,从而以扬长避短的方式实现了对负载组分的分离与检定,是目前我国生     

气相色谱-质谱联用法同时测定饮用水源水中33种VOCs

气相色谱-质谱联用法充分结合了气相色谱和质谱的优点,在VOCs的测定中被广泛应用。本文利用气相色谱-质谱联用法对饮用水源水中的33种VOCs进行了测定,结论表明该方法检出限低、可靠性高,具有良好的应用成效。     

乙酸酐和三乙胺组合衍生在水产品中氯霉素测定的应用

正氯霉素广泛应用于动物传染性疾病的治疗,曾在水产养殖业中得到广泛的应用,但同时也带来了严重的残留问题,氯霉素能够抑制人体骨髓造血功能,引起贫血等。因此对水产品中的氯霉素的检测具有特殊意义。国内外文献报道氯霉素类药物的检测方法主要采用气相色谱法、气相色谱-质谱联用法和液相色谱-质谱联用法。气相色谱-质谱联用法和液相色谱-质谱联用法灵敏度高,但价格昂贵,一般基层实验室不配备这样的仪器,     

万寿菊花超临界萃取物气相色谱－质谱分析

结合气相色谱- 质谱联用法对万寿菊花超临界萃取物的挥发性成分进行分析。采用超临界二氧化碳提取分离万寿菊花中叶黄素脂肪酸酯,含量为20%。用气相色谱- 质谱联用技术分析超临界萃取物中的挥发性成分,鉴定出17 种化合物,其中香树脂素及其同分异构体占21.00%,甾醇类物质占10.79%,VE 占4.36%。     

食品中N-亚硝胺类化合物检测方法研究进展

N-亚硝胺类化合物是种强致癌物,主要介绍了N-亚硝胺类化合物的种类;食品中N-亚硝胺类化合物的危害;食品中N-亚硝胺类化合物国家检测限量要求;食品中N-亚硝胺类化合物的5种检测方法(气相色谱法、气相色谱-质谱联用法、气相色谱-热能分析仪联用法、高效液相色谱-质谱联用法、二次展开光解薄层层析法),并探讨各检测方法优缺点并展望未来检测方法发展趋势。     

油茶籽油与橄榄油化学成分研究

研究油茶籽油和橄榄油的化学成分,采用毛细管气相色谱-质谱联用法结合计算机检索对其进行分析和鉴定,用气相色谱面积归一化法测定各组分的相对百分含量.共鉴定出油茶籽油的9个化合物和橄榄油的10个化合物.研究结果表明,油茶籽油和橄榄油的化学成分和相对含量存在很大差异,其中油茶籽油中的十六烷酰胺和橄榄油中的α-法呢烯、硬脂酰胺、2-甘油单油酸酯均为首次分离报道.     

纺织品中五氯酚残留量检测方法的研究

概述了纺织品五氯酚(PCP)残留量的检测方法,包括分光光度法、高效液相色谱法(HPLC)、高效液相色谱/质谱联用法(HPLC/MS)、气相色谱法(GC)、气相色谱/质谱联用法(GC/MS)和免疫分析法等,总结了各种检测方法的优缺点,并提出了纺织用PCP残留检测的发展方向.     

烟用香精的极性偶合柱系统分析

为提高烟用香精分析结果的可靠性,针对在单柱气相色谱/质谱(GC/MS)上分离峰效果不佳或色谱图中有明显重叠峰的烟用香精,作者采用极性偶合柱系统GC/MS进行了定性分析,并优化分析条件,与单柱GC/MS分析结果进行比较。最后,比较了不同分析结果所得化学成分和品吸结果之间的对应关系。结果表明,极性偶合柱系统GC/MS比单柱GC/MS具有更强的分离能力,可定性的组分明显多于一维GC/MS,并且更符合该香精的评吸结果。这种分析方法有利于更全面地认识香精的化学成分,更准确地认识香精的组成与功能之间的关系。为增强加香配方研究的科学性、提高调香工作的效率提供有力的支持。     

多维气相色谱/质谱法快速测定卷烟烟气中的苯并(a)芘

自行组装了一套具有全自动和在线富集功能的大孔径-毛细柱多维气相色谱(MDGC)系统。应用该系统,开发了一种简便快速且准确的检测卷烟烟气苯并(a)芘的方法。收集在剑桥滤片上的烟气冷凝物用环己烷提取和浓缩后,不需要任何净化,可直接进行MDGC-MS-SIM分析。方法的重现性、回收率和检测限均令人满意。对不同配方和过滤嘴的卷烟样品进行了定量测定,对样品的测定结果进行了比较。      

Applicability of GC, GC/MS and liquid chromatography with tandem mass spectrometry to screening for 140 pesticides in agricultural products

The applicability of GC, GC/MS and liquid chromatography with tandem mass spectrometry (LC/MS/MS) to screening for 140 pesticides in agricultural products was examined. Validation of multi-residue screening methods for the determination of 88 pesticides in 12 crops (asparagus, cauliflower, burdock, carrot, broccoli, spinach, matsutake mushroom, orange, soybean, sesame, millet and tea) was done by GC and GC/MS. Of the 88 pesticides, 63 were obtained with recoveries in the range from 50 to 150% at the 0.1 microg/g level in the 12 crops. Applicability of the official methods in Japan to 74 pesticides, including 22 pesticides with low recovery (< 50%) by GC or GC/MS analysis, was also examined by LC/MS/MS. LC/MS/MS acquisition parameters were established for 67 pesticides in positive and negative electrospray ionization (ESI) modes. Of 67 pesticides validated in 7 crops using LC/MS/MS at the 0.1 microg/g level, 44 showed recoveries in the range from 50 to 150%. The occurrence of matrix interference in LC/MS/MS can lead to false-positive detection of MCPA in spinach, cabbage and orange and false-negative detection of four pesticides in orange, spinach, apple and unpolished rice. Good linearity was observed in the studied ranges by GC, GC/MS (r > 0.990) and LC/MS/MS (r > 0.995). Of the total of 140 pesticides validated by GC, GC/MS and LC/MS/MS, 107 were newly recognized as suitable subjects for screening.     

Differentiation of wines according to grape variety using multivariate analysis of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometric detection data

Headspace solid-phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry detection (GC×GC/TOFMS) was used to analyse the volatiles in five types of wines elaborated with grapes of Cabernet Sauvignon, Merlot, Chardonnay, Sauvignon Blanc and Pinot Noir varieties. Fisher ratio, principal component analysis (PCA) and stepwise linear discriminant analysis (SLDA) were used to develop a discriminant model and, as a result, 12 volatile compounds enabled differentiation and classification of wines according to grape cultivars. A detailed examination of GC×GC/TOFMS data showed that the use of one-dimensional gas chromatography with a mass spectrometric detector (1D-GC/MS) would probably result in misidentification of some of these 12 compounds, as they showed partial coelution with other components in the first chromatographic dimension.     

Study on the determination of pesticide residues in crops by ion-trap GC/MS/MS

Ion-trap GC/MS/MS was evaluated for the multi-residue determination of pesticides in agricultural products. Matrices were extracted from samples (spinach, carrot, onion and brown rice) with acetone and submitted to gel permeation chromatography, followed by a clean-up step through a graphite carbon cartridge. Thirty-five pesticides were added to either matrix, and analyzed by GC/MS/MS. Detection limits of pesticides by GC/MS/MS was almost the same as those by GC/MS (SIM). Coefficients of variation of peak area in 5 measurements of each pesticide at 0.1 microgram/mL or 0.05 microgram/mL with or without matrices were mostly acceptable, though those of 20 pesticides out of 35 were higher than 10% at a concentration of 0.02 microgram/mL. It was indicated that matrix artifacts, which interfere with GC/MS-Scan analysis, could be eliminated in some cases by using GC/MS/MS.     

Screening for estrogen residues in calf urine: comparison of a validated yeast estrogen bioassay and gas chromatography-tandem mass spectrometry.

Within the European Union, the control for residues of illegal hormones in food-producing animals is based on urine analysis for a few target analytes using gas chromatography/mass spectrometry and/or liquid chromatography-tandem mass spectrometry. Recently, we developed a robust yeast bioassay screening tool for estrogens, which was validated as a qualitative screening method in accordance with EC decision 2002/657/EC. In this study, we present long-term performance data and a comparison of urine data obtained with this bioassay, and data from an established gas chromatography-tandem mass spectrometry (GC/MS/MS) confirmatory analysis method. More than 120 calf urine samples from a controlled reference experiment were analysed using both protocols. According to the GC/MS/MS method, only the natural estrogens 17alpha-estradiol and estrone were present in the non-compliant samples. The bioassay was less sensitive than GC/MS/MS for the relatively weak estrogenic compound 17alpha-estradiol, in accordance with expectations. Assuming that application of the mass spectrometric method is considered beyond reasonable doubt, the bioassay performed very well: only 5.6% of the calf urine samples found compliant in GC/MS/MS were screened false suspect in the bioassay screening method. The bioassay results of non-compliant urine samples under routine conditions were as predicted, taking into account the relative estrogenicity of the natural estrogens 17alpha-estradiol and estrone vs. 17beta-estradiol. Only one sample was screened false negative for 17alpha-estradiol and estrone. Application of this fast and simple estrogen bioassay in routine surveillance and control can significantly reduce GC/MS/MS sample workload and allow higher percentages of animals to be screened for potential hormone abuse.     

GC/MS法同时检测无烟气烟草制品中的1,2-丙二醇、丙三醇和三甘醇

为了准确测定无烟气烟草制品中保润剂的含量,以1,4-丁二醇为内标建立了同时检测无烟气烟草制品中1,2-丙二醇、丙三醇、三甘醇的气相色谱/质谱/选择离子监测(GC/MS/SIM)方法,采用该方法和CORESTA推荐的GC/FID法测定了30个无烟气烟草制品样品,并将2种方法的检测结果进行了比较.结果表明:①该方法的检出限和定量限分别为1.25～2.75 μg/g和4.10-9.05 μg/mL,回收率89.3%～100.3%,相对标准偏差(RSD)1.16%～4.37%;②所测无烟气烟草制品中1,2-丙二醇、丙三醇、三甘醇的含量分别在0.011-40.817,0.024～39.044和0.012～0.099 mg/g之间;③GC/FID法检出13个样品中舍1,2-丙二醇,检出率43.3%;14个样品中含丙三醇,检出率46.7%,其中能够准确定量的有9个样品;未检出三甘醇;④GC/MS/SIM法检出29个样品中含1,2-丙二醇,检出率96.7%,其中能够准确定量的有16个样品;28个样品中含丙三醇,检出率93.3%,其中能够准确定量的有25个样品;21个样品中含三甘醇,检出率70.0%,其中能够准确定量的有11个样品;⑤GC/FID和GC/MS/SIM法共同检出的13个样品中的1,2-丙二醇含量和9个样品的丙三醇含量的皮尔逊(Pearson)相关系数均大于0.99,概率P值均小于显著性水平0.05,配对t检验概率P值均大于显著性水平0.05.结论:两种方法的定量结果一致,但GC/MS/SIM法灵敏度更高,定性更准确,GC/MS/SIM法更适合无烟气烟草制品中1,2-丙二醇、丙三醇、三甘醇的定性定量分析.     

Determination of low-level pesticide residues in agricultural products by ion-trap GC/MS/MS

The objective of this study was to elucidate the utility of ion-trap GC/MS/MS for the analysis of pesticides in extracted matrices from various agricultural products. Identification and quantitative analysis of pesticides in matrices were performed by quadrupole GC/MS and ion-trap GC/MS/MS. Chlorpyrifos was added to the matrix of spinach, soybean in the pod or corn, and aldrin, dieldrin, endrin, alpha-BHC, beta-BHC, gamma-BHC, delta-BHC, p,p'-DDD, p,p'-DDE, o,p'-DDT and p,p'-DDT were added to each matrix of green tea, black tea or oolong tea. Although most of the pesticides in the matrix could not be determined by quadrupole GC/MS-Scan analysis at 0.1 microgram/mL, every pesticide was identified from the mass spectrum using ion-trap GC/MS/MS at the same concentration. The quantitation limit of every pesticide in each matrix by ion-trap GC/MS/MS analysis was higher than that by GC/MS-SIM analysis. The calibration curves obtained by GC/MS/MS were linear in the range of 0.01-0.25 microgram/mL of each pesticide. The recoveries of each pesticide from four kinds of samples spiked at the levels of 0.01 ppm to 0.02 ppm in extracts were 61.2-138.3% with SD values in the range from 1.2 to 15.4%. This study revealed that ion-trap GC/MS/MS was useful for the identification and quantitative analysis of low-level pesticides residues in matrices of agricultural products.     

Multiresidue method for determination of pesticides in fruits and vegetables by GC/MS (SCAN) and LC/MS (SIM)

A rapid multiresidue method has been developed for determination of many pesticides in fruits and vegetables using GC/MS and LC/MS. The method of analysis was the same as that reported by Kakimoto et al. in 2003 except for the use of LC/MS. Good recoveries in the range of 70-120% were obtained for 70 (32 by GC/MS, 38 by LC/MS) of 113 pesticides spiked at 0.1 microg/g into fruits and vegetables. For screening purposes, the method could be appiled to 82 pesticides. Considering the report by Kakimoto et al. in 2004, 177 pesticides were suitable for screening by this method. The limits of detection were 0.001-0.015 microg/g (by GC/MS) and < 0.001-0.010 microg/g (by LC/MS). The calibration curves were linear for most pesticides, with correlation coefficients of 0.976-1.000 (by GC/MS) and 0.968-1.000 (by LC/MS). The values obtained for fruits and vegetables naturally contaminated with pesticides by this method were nearly equal to those by the official method.     

Analytical method validation for terbutryn using gas chromatography/ion trap,gas chromatography/mass selective detector,and liquid chromatography/triple quadrupole mass spectrometers

Food Science and Biotechnology - Analytical methods including solvent extraction followed by gas chromatography/ion-trap (GC/IT) with scan and MS/MS mode, a GC/mass selective detector (GC/MSD), and...