超高效液相色谱法同时测定膨胀烟丝中3种糠醛类化合物
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摘要
粉碎后的膨胀烟丝样品(约1g)用乙腈-二氯甲烷(1+1)混合液20 mL超声提取40min,取适量上清液在10 000r·min~(-1)转速下离心15min,过0.22μm的滤膜。采用超高效液相色谱法同时测定滤液中3种糠醛类化合物的含量。以ACCQ-TAG~(TM)ULTRA C_(18)色谱柱为分离柱,以乙腈(1+9)溶液为流动相,在检测波长284nm处进行测定。3种糠醛类化合物的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3s)为0.012～0.015 mg·L~(-1),测定下限(10s)为0.040～0.050mg·L~(-1)。方法用于膨胀烟丝样品的分析,加标回收率为76.1%～102%,测定值的相对标准偏差(n=5)为3.2%～4.9%。
The crushed sample(about 1 g) of expanded tobacco was extracted ultrasonically for 40 min with 20 mL of the mixture of acetonitrile and dichloromethane(1+1).Appropriate supernatant was centrifugated for 15 min at the speed of 10 000 r·min~(-1) and filtered on 0.22μm membrane.UHPLC was applied to the simultaneous determination of 3 furfural compounds in the filtrate.ACCQ-TAG~(TM)ULTRA C_(18) chromatographic column was used as separation column,and acetonitrile(1+9) solution was used as mobile phase.Detection at 284 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of the 3 furfural compounds were kept in definite ranges,with detection limits(3s) in the range of 0.012-0.015 mg·L~(-1) and lower limits of determination(10s) in the range of 0.040-0.050 mg·L~(-1).The proposed method was applied to the analysis of the sample of expanded cut tobacco,giving values of recovery found by standard addition method and RSDs(n=5) of determined values in the ranges of 76.1%-102% and 3.2%-4.9% respectively.
The crushed sample(about 1 g) of expanded tobacco was extracted ultrasonically for 40 min with 20 mL of the mixture of acetonitrile and dichloromethane(1+1).Appropriate supernatant was centrifugated for 15 min at the speed of 10 000 r·min~(-1) and filtered on 0.22μm membrane.UHPLC was applied to the simultaneous determination of 3 furfural compounds in the filtrate.ACCQ-TAG~(TM)ULTRA C_(18) chromatographic column was used as separation column,and acetonitrile(1+9) solution was used as mobile phase.Detection at 284 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of the 3 furfural compounds were kept in definite ranges,with detection limits(3s) in the range of 0.012-0.015 mg·L~(-1) and lower limits of determination(10s) in the range of 0.040-0.050 mg·L~(-1).The proposed method was applied to the analysis of the sample of expanded cut tobacco,giving values of recovery found by standard addition method and RSDs(n=5) of determined values in the ranges of 76.1%-102% and 3.2%-4.9% respectively.
引文
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[14] YIN F,ZHANG X M,SONG S Q,et al.Identification of aroma types and their characteristic volatile compounds of Chinese faint-scent cigarettes based on descriptive sensory analysis and GC-MS and partial least squares regression[J].European Food Research and Technology,2016,242(6):869-880.
[15] J?BSTL D,HUS?Y T,ALEXANDER J,et al.Analysis of 5-hydroxymethyl-2-furoic acid(HMFA)the main metabolite of alimentary 5-hydroxymethyl-2-furfural(HMF)with HPLC and GC in urine[J].Food Chemistry,2010,123(3):814-818.
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[17] VíCTOR-ORTEGA M D,LARA F J, GARCíA-CAMPA?A A M,et al.Evaluation of dispersive liquid-liquid microextraction for the determination of patulin in apple juices using micellar electrokinetic capillary chromatography[J].Food Control,2013,31(2):353-358.
[18]赵颖,张璐欣,李越,等.5-羟甲基糠醛的研究概况[J].医学综述,2016,22(17):3431-3434.
[19] YC/T 31-1996烟草及烟草制品试样的制备及水分的测定烘箱法[S].
[20] SUN S H,WANG H,XIE J P,et al.Simultaneous determination of rhamnose,xylitol,arabitol,fructose,glucose,inositol,sucrose,maltose in jujube(Zizyphus jujube Mill.)extract:comparison of HPLC-ELSD, LC-ESI-MS/MS and GC-MS[J].Chemistry Central Journal,2016,10:1-9.
[21]牛勇,邹鹏,舒俊生,等.二氧化碳膨胀处理对烟丝部分香味成分的影响[J].烟草科技,2014,47(9):57-60.
[22]李晓,王建民,李华杰,等.微波烘丝前后烟丝中主要中性香味成分分析[J].烟草科技,2006,39(2):13-17.
[2] MAURON J.The Maillard reaction in food;a critical review from the nutritional standpoint[J].Progress in Food&Nutrition Science,1981,5(1/6):5-35.
[3] ABU-BAKAR N B,MAKAHLEH A,SAAD B.Vortex-assisted liquid-liquid microextraction coupled with high performance liquid chromatography for the determination of furfurals and patulin in fruit juices[J].Talanta,2014,120:47-54.
[4] MICHAIL K,MATZI V,MAIER A,et al.Hydroxymethylfurfural:An enemy or a friendly xenobiotic?A bioanalytical approach[J].Analytical and Bioanalytical Chemistry,2007,387(8):2801-2814.
[5] FOO WONG Y,MAKAHLEH A,AL AZZAM K M,et al. Micellar electrokinetic chromatography method for the simultaneous determination of furanic compounds in honey and vegetable oils[J].Talanta,2012,97:23-31.
[6]王歌,曾睿,邱瑞霞,等.5-羟甲基糠醛与氨基酸反应形成的风味物质[J].食品与机械,2018,34(8):1-4.
[7]徐禄江,陆强,姚倩,等.选择性热化学催化转化果糖制备5-甲基糠醛和糠醛[J].科学通报,2015,60(16):1530-1537.
[8] ADAMS T B,DOULL J,GOODMAN J I,et al.The FEMA GRAS assessment of furfural used as a flavour ingredient[J].Food and Chemical Toxicology,1997,35(8):739-751.
[9]张玉玉,宋弋,李全宏.食品中糠醛和5-羟甲基糠醛的产生机理、含量检测及安全性评价研究进展[J].食品科学,2012,33(5):275-280.
[10]叶楠,肖作兵,刘强,等.气质联用-选择离子扫描测定卷烟主流烟气中糠醛的含量[J].食品工业科技,2012,33(9):366-368.
[11] CAI J B,LIU B Z,LING P,et al.Analysis of free and bound volatiles by gas chromatography and gas chromatography-mass spectrometry in uncased and cased tobaccos[J].Journal of Chromatography A,2002,947:267-275.
[12] DING Y,ZHU L J,LIU S M,et al.Analytical method of free and conjugated neutral aroma components in tobacco by solvent extraction coupled with comprehensive two-dimensional gas chromatographytime-of-flight mass spectrometry[J].Journal of Chromatography A,2013,1280:122-127.
[13]任呼博,别振英,朱友,等.超高效液相色谱法同时测定烟用香精料液中的糠醛、5-羟甲基糠醛与5-甲基糠醛[J].分析测试学报,2015,34(11):1291-1295.
[14] YIN F,ZHANG X M,SONG S Q,et al.Identification of aroma types and their characteristic volatile compounds of Chinese faint-scent cigarettes based on descriptive sensory analysis and GC-MS and partial least squares regression[J].European Food Research and Technology,2016,242(6):869-880.
[15] J?BSTL D,HUS?Y T,ALEXANDER J,et al.Analysis of 5-hydroxymethyl-2-furoic acid(HMFA)the main metabolite of alimentary 5-hydroxymethyl-2-furfural(HMF)with HPLC and GC in urine[J].Food Chemistry,2010,123(3):814-818.
[16] GASPAR E M S M,LOPES J F.Simple gas chromatographic method for furfural analysis[J].Journal of Chromatography A,2009,1216:2762-2767.
[17] VíCTOR-ORTEGA M D,LARA F J, GARCíA-CAMPA?A A M,et al.Evaluation of dispersive liquid-liquid microextraction for the determination of patulin in apple juices using micellar electrokinetic capillary chromatography[J].Food Control,2013,31(2):353-358.
[18]赵颖,张璐欣,李越,等.5-羟甲基糠醛的研究概况[J].医学综述,2016,22(17):3431-3434.
[19] YC/T 31-1996烟草及烟草制品试样的制备及水分的测定烘箱法[S].
[20] SUN S H,WANG H,XIE J P,et al.Simultaneous determination of rhamnose,xylitol,arabitol,fructose,glucose,inositol,sucrose,maltose in jujube(Zizyphus jujube Mill.)extract:comparison of HPLC-ELSD, LC-ESI-MS/MS and GC-MS[J].Chemistry Central Journal,2016,10:1-9.
[21]牛勇,邹鹏,舒俊生,等.二氧化碳膨胀处理对烟丝部分香味成分的影响[J].烟草科技,2014,47(9):57-60.
[22]李晓,王建民,李华杰,等.微波烘丝前后烟丝中主要中性香味成分分析[J].烟草科技,2006,39(2):13-17.