顶空衍生固相微萃取测定大米中醛类物质

郝俊光; 杨理章; 樊伟; 陆健; 董建军; 尹花; 余俊红; 闫鹏; 陈华磊; 田玉红

doi:10.13386/j.issn1002-0306.2014.09.050

顶空衍生固相微萃取测定大米中醛类物质

郝俊光¹,
杨理章^1,2,3,4,
樊伟^1,2,
陆健^2,3,4,
董建军¹,
尹花¹,
余俊红¹,
闫鹏¹,
陈华磊¹,
田玉红¹

1. 啤酒生物发酵工程国家重点实验室
2. 江南大学生物工程学院
3. 江南大学粮食发酵工艺与技术国家工程实验室
4. 江南大学工业生物技术教育部重点实验室

基金项目:

国家973项目(2012CB723707)；江苏高校优势学科建设工程资助项目；

详细信息

作者简介:
郝俊光 (1971-) , 男, 博士, 工程技术应用研究员, 研究方向:啤酒酿造关键技术和风味调控技术。;

中图分类号: O657.63;TS210.7
计量
- 文章访问数: 0130
- HTML全文浏览量: 026
- PDF下载量: 0263
出版历程
- 收稿日期: 2013-09-04

Analysis of aldehydes in rice using solid-phase microextraction with on-fiber derivatization

State Key Laboratory of Biological Fermentation Engineering of Beer, Technical Center of Tsingtao Brewery Co.Ltd.
School of Biotechnology, Jiangnan University
National Engineering Laboratory for Cereal Fermentation Technology, Jiangnan University
The Key Laboratory of Industrial Biotechnology, Ministry of Education, Schoolof Biotechnology, Jiangnan University

摘要

摘要: 本研究利用顶空衍生固相微萃取气相色-谱质谱建立了定量分析大米中醛类物质的方法。通过研究萃取头、衍生剂量、萃取温度和萃取时间对醛类物质检测的影响,确定了顶空衍生固相微萃取的最佳条件:65μm PDMS/DVB在装有10mL 60mg/L邻-五氟苄基羟胺溶液的顶空瓶中40℃吸附衍生试剂20min,之后萃取头换至装有样品的顶空瓶中40℃衍生萃取80min。所建方法的9种醛类物质在各自线性范围内标准曲线线性良好,R2均大于0.99,相对标准偏差在5.0%⁷.5%（n=5）,检出限在0.010⁰.695μg/kg,加标回收率在77.9%¹24.2%。本方法可依次自动完成萃取头的衍生试剂吸附以及醛类物质萃取、进样、分离和测定,检测效率高,适用于大米醛类物质的日常大量检测。对大米样品的醛类物质和品评结果进行相关性分析,发现戊醛和己醛是评价大米品质的重要指标。
- 衍生 /
- 顶空固相微萃取 /
- 气相色谱质谱 /
- 醛类物质 /
- 大米
Abstract: A simple, practical and sensitive method based on solid- phase micro- extraction ( SPME) with on- fiber derivatization coupled with gas chromatography mass spectrometry ( GC- MS) was developed for the analysis of aldehydes in rice.The major factors which affect the effect of SPME, such as type of the fiber, quantity of derivatization reagent, temperature and time of extraction were studied.The results showed that a 65μm PDMS/DVB fiber coating with the 10mL 60mg /L O- ( 2, 3, 4, 5, 6- pentafluorobenzyl) - hydroxylamine for 20min at 40℃ in the headspace of derivatization-reagent-vial followed by extracting for 80min at 40℃ in sample vial headspace was the optimum condition of SPME with on- fiber derivatization.The 9 aldehydes were found to be linear in the validated range with correction coefficients ( R2) better than 0.99.The limitations of detection of the method were 0.010⁰.695μg /kg in rice while the relative standard deviations ( RSD) were 5.0% ⁷.5% ( n = 5) .The recoveries of aldehydes were found to be 77.9% ~ 124.2%.This consecutive operation of this method, namely coating with the derivatizing reagent, extraction of aldehydes, injection and detection, could automatically completed on line, which made it efficient and suitable for routine analysis of rice aldehydes.Base on correlation anlysis between aldehydes and sensory evaluation scores of rice samples, it was found that hexanal and pentanal were important indices to rice quality.
- derivatization /
- headspace solid phase micro-extraction /
- GC-MS /
- aldehyde /
- rice

HTML全文

参考文献(16)

[1]	Champagne E T.Rice aroma and flavor:a literature review[J].Journal of Cereal Chemistry, 2008, 85 (4) :445-454.
[2]	陈玮, 李喜宏, 郭红莲, 等.天津大米超长期贮藏的醛系物积累与调控研究[J].中国粮油学报, 2007, 22 (6) :139-141.
[3]	Zhou Z, Robards K, Helliwell S, et al.Ageing of stored rice:changes in chemical and physical attributes[J].Journal of Cereal Science, 2002, 35 (1) :65-78.
[4]	Tsugita T, Ohta T, Kato H.Cooking flavor and texture of rice stored under different conditions[J].Agricultural and Biological Chemistry, 1983, 47 (3) :543-549.
[5]	林家永, 高艳娜, 吴胜芳, 等.顶空固相微萃取-气质联用法分析稻谷挥发性成分[J].食品科学, 2009, 30 (20) :277-282.
[6]	Tananuwong K, Lertsiri S.Changes in volatile aroma compounds of organic fragrant rice during storage under different conditions[J].Journal of the Science of Food and Agriculture, 2010, 90 (10) :1590-1596.
[7]	Vesely P, Lusk L, Basarova G, et al.Analysis of aldehydes in beer using solid-phase microextraction with on-fiber derivatization and gas chromatography/mass spectrometry[J].Journal of Agricultural and Food Chemistry, 2003, 51 (24) :6941-6944.
[8]	蔡建梅, 穆晓燕.粳稻谷及大米新陈鉴定方法探讨[J].粮油食品科技, 2012, 20 (3) :31-32.
[9]	Ma J, Xiao R, Li J, et al.Headspace solid-phase microextraction with on-fiber derivatization for the determination of aldehydes in algae by gas chromatography-mass spectrometry[J].Journal of Separation Science, 2011, 34 (12) :1477-1483.
[10]	Naeko S, Tomoo N, Katsumi S, et al.Analysis of aldehydes in water by head space-GC/MS[J].Jouranl of Health Science, 2001, 47 (1) :21-27.
[11]	白栋强, 王若兰.脂肪氧化酶在稻米储藏和加工中的应用[J].粮食科技与经济, 2003 (4) :44-45.
[12]	Ramezanzadeh F M, Rao R M, Windhauser M, et al.Prevention of oxidative rancidity in rice bran during storage[J].Journal of Agricultural and Food Chemistry, 1999, 47 (8) :2997-3000.
[13]	Vanderhaegen B, Neven H, Verachtert H, et al.The chemistry of beer aging-a critical review[J].Food Chemistry, 2006, 95 (3) :357-381.
[14]	Stashenko E E, Martínez J R.Derivatization and solid-phase microextraction[J].Trends in Analytical Chemistry, 2004, 23 (8) :553-561.
[15]	Baert J J, De Clippeleer J, Hughes P S, et al.On the origin of free and bound staling aldehydes in beer[J].Journal of Agricultural and Food Chemistry, 2012, 60 (46) :11449-11472.
[16]	张玉荣, 高艳娜, 林家勇, 等.顶空固相微萃取-气质联用分析小麦储藏过程中挥发性成分变化[J].分析化学, 2010, 38 (7) :953-957.