气相色谱-质谱法检测日用香精中3种禁用麝香物质
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摘要
建立了一种同时检测日用香精中葵子麝香、伞花麝香和西藏麝香等3种禁用麝香类物质的气相色谱-质谱(GCMS)方法,采用外标法结合离子(SIM)扫描对3种物质进行了定性定量分析。结果表明:该方法在质量浓度0.001到0.500 mg/mL范围内的响应线性关系良好,相关系数均大于0.9980;检出限为0.005μg/mL(S/N≥3)。在100μg/mL和200μg/ml加标浓度下,三种麝香的回收率在80%至120%之间,精密度<10%,重复性较好。该方法满足分析检测要求,可用于日用香精中葵子麝香、伞花麝香和西藏麝香的定性定量分析。同时将此方法应用到不同薄荷香精样品中3种禁用麝香类物质的检测,未检测到目标化合物。
A gas chromatography-mass spectrometry (GC-MS) method for determination of prohibited musk ambrette, moskene and musk tibetene in fragrances was established. The method was validated in terms of linearity, limits of detection, recovery and precision. The results showed that the method had great linearity (>0.9980) with the concentration from 0.001 to 0.500 mg/mL. And the limits of detection (LOD) was 0.005 μg/mL for all of these three target compounds. Besides, the recovery was from 80% to 120% with relative standard deviation (RSD) below 10% at 100 μg/mL and 200 μg/mL quality control concentration levels. The method met the requirement of trace detection, which can be applied in testing of musk ambrette, moskene and musk tibetene in fragrances. When it was applied to detect these three components in different mint fragrance samples, none of them was detected out.
A gas chromatography-mass spectrometry (GC-MS) method for determination of prohibited musk ambrette, moskene and musk tibetene in fragrances was established. The method was validated in terms of linearity, limits of detection, recovery and precision. The results showed that the method had great linearity (>0.9980) with the concentration from 0.001 to 0.500 mg/mL. And the limits of detection (LOD) was 0.005 μg/mL for all of these three target compounds. Besides, the recovery was from 80% to 120% with relative standard deviation (RSD) below 10% at 100 μg/mL and 200 μg/mL quality control concentration levels. The method met the requirement of trace detection, which can be applied in testing of musk ambrette, moskene and musk tibetene in fragrances. When it was applied to detect these three components in different mint fragrance samples, none of them was detected out.
引文
[1]左壮.天然麝香化学成分研究概况[J].长春中医药大学学报,1987(3):40-41.
[2]吕建国,韩恩硕.天然麝香香气成份的研究[J].甘肃科技,1994(3):38-39.
[3]朱秀嫒,王文杰,徐桂芳,等.麝香的药理研究Ⅱ.麝香及其有效成分的抗炎作用[J].药学学报,1988(6):406-410.
[4]孙蓉,王任卿,于晓,等.麝香的化学与药理研究进展[J].药学研究,2005,24(5):296-297.
[5]郝吉福,程怡.麝香的药理学研究概况[J].时珍国医国药,2004,15(4):248-249.
[6]王婷,宋怀燕,张文明.麝香开窍颗粒对小鼠记忆损害的影响[J].实验动物科学,2002,19(3):17-19.
[7]王景超.麝香注射液治疗急性脑血管病意识障碍108例[J].陕西中医,2005,26(2):108-109.
[8]苏泽礼,王庆.新生儿麝香中毒致多脏器功能损害1例[J].中国现代应用药学,2001,18(1):78.
[9]吕济民.英国对人工麝香含致癌物的产品进行调查[J].中国标准导报,2000(1):23.
[10]周启星,王美娥,范飞,等.人工合成麝香的环境污染、生态行为与毒理效应研究进展[J].环境科学学报,2008,28(1):1-11.
[11]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.日用香精:GB/T 22731[S].北京:中国标准出版社,2008.
[12]张皓冰,陶奕,洪筱坤,等.气相色谱/质谱(GC/MS)联用测定麝香中甾体成分的研究[J].中成药,2005,27(1):79-83.
[13]张皓冰,何昱,贾国惠,等.气相色谱/质谱(GC/MS)联用技术对麝香的多成分含量分析[J].中成药,2002,24(11):868-871.
[14]吴春英,白鹭,陆文龙,等.气相色谱-串联质谱法同时快速检测环境水样中11种合成麝香[J].分析科学学报,2016,32(2):188-192.
[15]QIN Z,PANG X,CHEN D,et al.Evaluation of Chinese tea by the electronic nose and gas chromatography-mass spectrometry:Correlation with sensory properties and classification according to grade level[J].Food Research International,2013,53(2):864-874.
[16]MAYR CM,Capone DL,Pardon KH,et al.Quantitative analysis by GC-MS/MS of 18 aroma compounds related to oxidative off-flavor in wines[J].Journal of Agricultural&Food Chemistry,2015,63(13):3394-3401.
[17]俞波,郭希圣.麝香甾体成分的高效液相色谱法研究[J].中草药,1989(11):11-14.
[18]王雪莹,陆舍铭,朱丽,等.超高效液相色谱法同时测定烟用香精中的蛇床子素和二氢欧山芹醇当归酸酯[J].香料香精化妆品,2012(1):1-6.
[19]李晶,徐济仓,李雪梅,等.超高效液相色谱法同时测定香精香料中14种禁限用物质[J].色谱,2012,30(8):816-821.
[20]ZENG Y,LUO JY,FAN YM,et al.Detection of flavor components in ethanol extract from kelp using GC-MSmethod[J].Food Science&Technology,2015,40(10):279-283.
[21]LI L,ZHENG L,LIU X.Analysis of jasmin fragrance isolated with solid phase microextraction by GC-MS[J].Chemical Analysis&Meterage,2006,15(2):37-39.
[22]LISKO JG,STANFILL SB,WASTON CH.Quantitation of ten flavor compounds in unburned tobacco products[J].Analytical Methods Advancing Methods&Applications.2014,6(13):4698-4704.
[23]WU P,ZHANG L,SHEN X,et al.Determination of ethyl carbamate in chinese yellow rice wine by diatomaceous earth extraction and GC/MS method[J].Journal of Aoac International.2015,98(3):834-838.
[24]ALAIN C,DANIEL J,CHRISTOPHE M,et al.GC-MSquantitation of fragrance compounds suspected to cause skin reactions.1[J].Journal of Agricultural&Food Chemistry.2003,51(22):6398-6403.
[25]DESMEDT B,CANFYN M,PYPE M,et al.HS-GC-MSmethod for the analysis of fragrance allergens in complex cosmetic matrices[J].Talanta,2015,131:444-451.
[26]KALOUSTIAN J,MIKAIL C,EL-MOSELHY T,et al.GC-MS analysis of allergens in plant oils meant to cosmetics[J].OCL-Oleagineux Corps Gras Lipides.2007,14(2):110-115.
[27]XIAO Zuobing,FAN Binbin,NIU Yunwei,et al.Characteriztion of odor-active compounds of various chrysanthemum essential oils by gas chromatography-olfactometry,gas chromatagraphymass spectrometry and their correlation with sensory attributes[J].Journal of Chromatography B,2016,1009:152-162.
[28]王素娟,赵敏,秦云华,等.气相色谱-质谱法测定食用香精中的6种化合物[J].理化检验-化学分册,2015,51(8):1140-1142.
[2]吕建国,韩恩硕.天然麝香香气成份的研究[J].甘肃科技,1994(3):38-39.
[3]朱秀嫒,王文杰,徐桂芳,等.麝香的药理研究Ⅱ.麝香及其有效成分的抗炎作用[J].药学学报,1988(6):406-410.
[4]孙蓉,王任卿,于晓,等.麝香的化学与药理研究进展[J].药学研究,2005,24(5):296-297.
[5]郝吉福,程怡.麝香的药理学研究概况[J].时珍国医国药,2004,15(4):248-249.
[6]王婷,宋怀燕,张文明.麝香开窍颗粒对小鼠记忆损害的影响[J].实验动物科学,2002,19(3):17-19.
[7]王景超.麝香注射液治疗急性脑血管病意识障碍108例[J].陕西中医,2005,26(2):108-109.
[8]苏泽礼,王庆.新生儿麝香中毒致多脏器功能损害1例[J].中国现代应用药学,2001,18(1):78.
[9]吕济民.英国对人工麝香含致癌物的产品进行调查[J].中国标准导报,2000(1):23.
[10]周启星,王美娥,范飞,等.人工合成麝香的环境污染、生态行为与毒理效应研究进展[J].环境科学学报,2008,28(1):1-11.
[11]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.日用香精:GB/T 22731[S].北京:中国标准出版社,2008.
[12]张皓冰,陶奕,洪筱坤,等.气相色谱/质谱(GC/MS)联用测定麝香中甾体成分的研究[J].中成药,2005,27(1):79-83.
[13]张皓冰,何昱,贾国惠,等.气相色谱/质谱(GC/MS)联用技术对麝香的多成分含量分析[J].中成药,2002,24(11):868-871.
[14]吴春英,白鹭,陆文龙,等.气相色谱-串联质谱法同时快速检测环境水样中11种合成麝香[J].分析科学学报,2016,32(2):188-192.
[15]QIN Z,PANG X,CHEN D,et al.Evaluation of Chinese tea by the electronic nose and gas chromatography-mass spectrometry:Correlation with sensory properties and classification according to grade level[J].Food Research International,2013,53(2):864-874.
[16]MAYR CM,Capone DL,Pardon KH,et al.Quantitative analysis by GC-MS/MS of 18 aroma compounds related to oxidative off-flavor in wines[J].Journal of Agricultural&Food Chemistry,2015,63(13):3394-3401.
[17]俞波,郭希圣.麝香甾体成分的高效液相色谱法研究[J].中草药,1989(11):11-14.
[18]王雪莹,陆舍铭,朱丽,等.超高效液相色谱法同时测定烟用香精中的蛇床子素和二氢欧山芹醇当归酸酯[J].香料香精化妆品,2012(1):1-6.
[19]李晶,徐济仓,李雪梅,等.超高效液相色谱法同时测定香精香料中14种禁限用物质[J].色谱,2012,30(8):816-821.
[20]ZENG Y,LUO JY,FAN YM,et al.Detection of flavor components in ethanol extract from kelp using GC-MSmethod[J].Food Science&Technology,2015,40(10):279-283.
[21]LI L,ZHENG L,LIU X.Analysis of jasmin fragrance isolated with solid phase microextraction by GC-MS[J].Chemical Analysis&Meterage,2006,15(2):37-39.
[22]LISKO JG,STANFILL SB,WASTON CH.Quantitation of ten flavor compounds in unburned tobacco products[J].Analytical Methods Advancing Methods&Applications.2014,6(13):4698-4704.
[23]WU P,ZHANG L,SHEN X,et al.Determination of ethyl carbamate in chinese yellow rice wine by diatomaceous earth extraction and GC/MS method[J].Journal of Aoac International.2015,98(3):834-838.
[24]ALAIN C,DANIEL J,CHRISTOPHE M,et al.GC-MSquantitation of fragrance compounds suspected to cause skin reactions.1[J].Journal of Agricultural&Food Chemistry.2003,51(22):6398-6403.
[25]DESMEDT B,CANFYN M,PYPE M,et al.HS-GC-MSmethod for the analysis of fragrance allergens in complex cosmetic matrices[J].Talanta,2015,131:444-451.
[26]KALOUSTIAN J,MIKAIL C,EL-MOSELHY T,et al.GC-MS analysis of allergens in plant oils meant to cosmetics[J].OCL-Oleagineux Corps Gras Lipides.2007,14(2):110-115.
[27]XIAO Zuobing,FAN Binbin,NIU Yunwei,et al.Characteriztion of odor-active compounds of various chrysanthemum essential oils by gas chromatography-olfactometry,gas chromatagraphymass spectrometry and their correlation with sensory attributes[J].Journal of Chromatography B,2016,1009:152-162.
[28]王素娟,赵敏,秦云华,等.气相色谱-质谱法测定食用香精中的6种化合物[J].理化检验-化学分册,2015,51(8):1140-1142.