褐煤的气相色谱/串联三重四极杆质谱鉴别检测方法
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摘要
基于传统褐煤鉴别方法操作复杂、定性结果主观影响较大等特点,探索并建立了褐煤的气相色谱/串联三重四极杆质谱鉴别方法(GC-MS/MS)。对煤炭样品采用丙酮溶液提取,提取液用气相色谱/串联三重四极杆质谱仪进行全扫描总离子流色谱和选择离子扫描及多反应监测扫描质谱(色谱和质谱)的采集分析。从总离子流图检测出褐煤的特征峰,结合特征峰的质荷比394.8/187、394.8/95、394.8/161、394.8/159.1对褐煤样品进行多反应监测模式(MRM)分析,使得定性分析更准确可靠。实验方法可广泛应用于煤炭中褐煤与其他种类煤炭区分的定性检测。
The operation of traditional identification method of lignite is complicated.Moreover,the qualitative results are greatly affected by the subjective factors.The identification and detection method of lignite by gas chromatography/triple quadrupole mass spectrometry(GC-MS/MS)was explored and established.The lignite sample was extracted with acetone solution.The extracting solution was collected and analyzed by full scanning total ion flow chromatography,selective ion scanning and multi-reaction monitoring scanning mass spectrometry(chromatography and mass spectrometry)using GC-MS/MS.The characteristic peaks of lignite were detected from total ion flow chromatorgraphy.According to the mass-to-charge ratios of characteristic peaks,i.e.,394.8/187,394.8/95,394.8/161 and 394.8/159.1,the lignite samples were analyzed at multi-reaction monitoring(MRM)mode to make the qualitative results more accurate and reliable.The proposed method could be widely used for the qualitative detection and identification of lignite from other types of coals.
The operation of traditional identification method of lignite is complicated.Moreover,the qualitative results are greatly affected by the subjective factors.The identification and detection method of lignite by gas chromatography/triple quadrupole mass spectrometry(GC-MS/MS)was explored and established.The lignite sample was extracted with acetone solution.The extracting solution was collected and analyzed by full scanning total ion flow chromatography,selective ion scanning and multi-reaction monitoring scanning mass spectrometry(chromatography and mass spectrometry)using GC-MS/MS.The characteristic peaks of lignite were detected from total ion flow chromatorgraphy.According to the mass-to-charge ratios of characteristic peaks,i.e.,394.8/187,394.8/95,394.8/161 and 394.8/159.1,the lignite samples were analyzed at multi-reaction monitoring(MRM)mode to make the qualitative results more accurate and reliable.The proposed method could be widely used for the qualitative detection and identification of lignite from other types of coals.
引文
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[16]盛文胜,李树岚,张彬.辨别真假蜂胶的一些方法[J].食品工业科技,2009,30(12):444-446.SHENG Wen-sheng,LI Shu-lan,ZHANG Bin.Some methods of identifying the true and false propolis[J].Science and Technology of Food Industry,2009,30(12):444-446.
[17]马纪伟,闰冬良.HPLC指纹图谱控制蜂胶质量[J].中国卫生检验杂志,2011,2l(9):2162-2163.MA Ji-wei,RUN Dong-liang.Study on HPLC fingerprint and quality control of propolis[J].Chinese Journal of Health Laboratory Technology,2011,2l(9):2162-2163.
[18]韩红祥,王维,陈雪松,等.应用HPLC-MS联用技术研究不同基源蜂胶指纹图谱[J].吉林中医药(Jilin Journal of Traditional Chinese Medicine),2011,31(12):1221-1223.
[19]周尊英,胡顺峰,王磊,等.煤炭贸易与检验[M].北京:中国标准出版社,2010:5-7.
[2]吴式瑜,王美丽.煤炭在中国能源的地位[J].煤炭加工与综合利用(Coal Processing &Comprehensive Utilization),2006,5(1):2-8.
[3]石文秀,张玉财,金管会.浅谈褐煤研究的必要性及褐煤的性质[J].化工进展,2012,31(s1):203-207.SHI Wen-xiu,ZHANG Yu-cai,JIN Guan-hui.The necessity of research on the lignite and lignite properties[J].Chemical Industry and Engineering Progress,2012,31(s1):203-207.
[4]梁永煌,游伟,章卫星.关于我国褐煤提质技术的应用现状及存在问题的解决方案[J].化肥设计,2013,50(6):1-9.LIANG Yong-huang,YOU Wei,ZHANG Wei-xing.Present application situation for quality upgrading technology of lignite in China and solution scheme of existing problems[J].Chemical Fertilizer Design,2013,50(6):1-9.
[5]董大啸,邵龙义.国际常见的煤炭分类标准对比分析[J].煤质技术,2015,3(2):54-58.DONG Da-xiao,SHAO long-yi.Comparative analysis of common coal quality classification standarads in the world[J].Coal Quality Technology,2015,3(2):54-58.
[6]王雪莹,王冰莹.煤及焦炭标准样品国内外发展概况[J].化学分析计量,2010,19(1):7-10.WANG Xue-ying,WANG Bing-ying.Development of coal&coke certified reference materials at home and abroad[J].Chemical Analysis and Meterage,2010,19(1):7-10.
[7]罗培培,傅雪海.我国褐煤共伴生资源分析及利用方向[J].煤炭科学技术,2012,40(12):118-121.LUO Pei-pei,FU Xue-hai.Analysis and utilization direction on associated resources of lignite in China[J].Coal Science and Technology,2012,40(12):118-121.
[8]尹立群.我国褐煤资源及其利用前景[J].煤炭科学技术,2004,32(8):12-15.YIN Li-qun.Lignite resources and utilization outlook in China[J].Coal Science and Technology,2004,32(8):12-15.
[9]傅雪海,路露,葛燕燕,等.我国褐煤资源及其物性特征[J].煤炭科学技术,2012,40(10):104-107.FU Xue-hai,LU Lu,GE Yan-yan,et al.China lignite resources and physical features[J].Coal Science and Technology,2012,40(10):104-107.
[10]周尊英,胡顺峰,王磊,等.煤炭贸易与检验[M].北京:中国标准出版社,2010:1-9.
[11]楮小立.化学计量学方法与分子光谱分析技术[M].北京:化学工业出版社,2011:31-123.
[12]李英华.煤质分析应用技术指南[M].北京:中国标准出版社,2010:229-230.
[13]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 2566—2010低煤阶煤的透光率测定方法[S].北京:中国标准出版社,2010.
[14]刘莉敏,郭军,米智慧,等.蜂胶样品乙醇提取物的UPLC-Q-TOF-MS指纹特征[J].食品科学,2014,35(18):96-98.LIU Li-min,GUO Jun,MI Zhi-hui,et al.UPLC-QTOF-MS fingerprint profiling of ethanol extracts of propolis[J].Food Science,2014,35(18):96-98.
[15]张翠萍,胡福良.蜂胶与杨树胶HPLC指纹图谱鉴别[J].中国食品学报,2011,11(1):222-225.ZHANG Cui-ping,HU Fu-liang.HPLC fingerprints in distinguishing propolis and poplar tree gum[J].Journal of Chinese Institute of Food Science and Technology,2011,11(1):222-225.
[16]盛文胜,李树岚,张彬.辨别真假蜂胶的一些方法[J].食品工业科技,2009,30(12):444-446.SHENG Wen-sheng,LI Shu-lan,ZHANG Bin.Some methods of identifying the true and false propolis[J].Science and Technology of Food Industry,2009,30(12):444-446.
[17]马纪伟,闰冬良.HPLC指纹图谱控制蜂胶质量[J].中国卫生检验杂志,2011,2l(9):2162-2163.MA Ji-wei,RUN Dong-liang.Study on HPLC fingerprint and quality control of propolis[J].Chinese Journal of Health Laboratory Technology,2011,2l(9):2162-2163.
[18]韩红祥,王维,陈雪松,等.应用HPLC-MS联用技术研究不同基源蜂胶指纹图谱[J].吉林中医药(Jilin Journal of Traditional Chinese Medicine),2011,31(12):1221-1223.
[19]周尊英,胡顺峰,王磊,等.煤炭贸易与检验[M].北京:中国标准出版社,2010:5-7.