《信阳毛尖茶中风味挥发物质的测定》团体标准编制说明

1工作简况1.1任务来源本项目是根据河南省食品工业协会2021年团体标准项目征集计划文件（豫食协[2021]03号），协会标准专业委员会进行了立项评审，符合立项条件，批准立项。项目批准立项文件为：豫食协[2021]04号，项目名称为：信阳毛尖茶风味挥发物质的测定。1.2主要工作过程标准制定计划下达后，在河南省食品工业协会标准专业委员会的领导下，主要起草单位认真落实和实施计划，牵头成立了标准起草工作组(以下简称“工作组”)。工作组在调查、收集、研究有关标准资料及分析、研究信阳毛尖茶风味挥发物质测定的基础上制定了检测技术路线。研制过程中，结合日常文献收集、摸底调研等前期工作基础，对相关内容进行验证、完善，建立了顶空气相色谱质谱测定方法。期间多次易稿修改，最终建立方法并组织2家单位进行实验室间验证，于2022年4月底完成了标准征求意见稿及其编制说明。2标准编制原则和主要内容的论据2.1标准编制原则本文件的编制以技术的先进性、标准的适用性、统一性、协调性为原则。标准的结构及编写方法按GB/T1.1-2020《标准化工作导则第1部分：标准化文件的结构和起草规则》。2.2标准主要技术内容方法规定了信阳毛尖茶风味挥发物质测定的顶空气相色谱质谱测定方法。本方法适用于信阳毛尖茶风味挥发物质的测定。2.3各项技术指标确立的原则和论据（1）检测技术路线信阳毛尖茶风味挥发物质测定方法比较多，经查阅文献，发现测定方法有热脱附气相色谱质谱法、液相色谱串接质谱法、气相色谱串接质谱法、顶空气相色谱高分辨质谱法等。其中，液相色谱串接质谱法测定低分子量香精种类少，灵敏度不足；热脱附气相色谱质谱法具有高灵敏度、快速、选择性好的特点，但是重现性较差，对吸附材料有特殊要求，方法普及性差；气相色谱串接质谱法对特定种类的香精具有高灵敏度和高重现性，但是需要对茶叶进行前处理，测定的化合物种类必须提前设定好方法。顶空气相色谱高分辨质谱法检测灵敏度高，但是没有公开公认的高分辨质谱库。采用顶空气相色谱质谱检测,能够对不同种类绿茶进行测定，化合物可使用NIST库进行识别定性，普及性强，操作简单。最终技术路线为：茶叶经粉碎过筛，采用顶空气相色谱质谱检测，使用NIST库进行识别定性，峰面积归一化法定量。茶叶样品处理绿茶按照GB/T18795-2012制样，称取待测绿茶2g于20mL顶空瓶中，密封，待测。色谱柱的选择本研究测定的是挥发性化合物，因此没有采用液体进样的色谱柱（通常膜厚0.25μm），采用挥发性化合物测定色谱柱DB-624UI色谱柱（30m×0.25mm×1.4μm）（膜厚1.4μm）对挥发性化合物分离效果好。升温程序优化研究比较了两种升温程序，升温程序A，40℃保持3min，以5℃/min升至260℃；升温程序B色谱柱初始温度40℃，保持1min，20℃/min到180℃，然后5℃/min到260℃保持5min；两种绿茶（代号p、x）在不同升温程序色谱图，见图1、2。图1升温程序A条件下绿茶p和绿茶x总离子流图图2升温程序A条件下绿茶p和绿茶x总离子流图升温程序A升温速度较慢，检测时间长，化合物分离效果好。升温程序B速度快，节省检测时间，但化合物分离效果差，尤其是2min～20min段化合物不能有效分离。考虑到定性是根据峰质谱图匹配，峰分不开会严重影响定性准确度，因此采用升温程序A。顶空温度选择加热温度是顶空进样重要的参数，改变加热温度能够影响顶空气中挥发物的种类和含量。研究选用了两种绿茶（代号p、x），在平衡温度50min条件下，进行温度单因素实验，加热温度分别为：60℃、80℃、100℃、120℃、140℃。总离子流图见图3。图3不同顶空加热温度下绿茶p和绿茶x总离子流图从图3可以看出，随加热温度提高，出峰数量整体呈现增加的趋势。但在较高温度下（140℃）出峰数量减少，减少的化合物主要在10min-20min，属于高沸点化合物。可能的原因是这些化合物在高温下参与化学反应，导致检测化合物数量较少。不同顶空加热温度下总离子流图积分提取化合物，积分时忽略峰面积＜最大峰面积5%的化合物，化合物提取数量见表2。表2化合物提取数量温度，℃绿茶x化合物数量，个绿茶p化合物数量，个6043802021100343612060601405148从表2中可以看出，温度120℃化合物数量最多，为60个。因此本部分选择最佳顶空温度为120℃。平衡时间的选择考察了顶空温度为120℃，绿茶x其中3个不同保留时间的化合物（保留时间3.3min、8.2min、12.1min），在30min、40min、50min、60min、70min的峰面积。将最大峰面积设为1，面积面积归一化计算3个化合物在不同温度下的峰面积。结果见图4图4不同顶空平衡时间对化合物峰面积响应影响从图4可以看出，随着平衡时间延长，化合物响应逐渐变大，在50min以后，化合物响应不再显著升高。考虑到过长加热时间浪费能源，延长检测时间。因此，选择平衡时间50min。方法学考察样品来源：信阳毛尖茶3批次，分别产自信阳云雾山、车云山、白龙潭。化合物种类：3批次茶叶中鉴定出匹配度≥80%化合物数量34种，精密度均在20%以内，详见表3。表3茶叶中挥发性化合物种类及精密度（RSD）序号cas号信阳毛尖（云雾山）信阳毛尖（车云山）信阳毛尖（白龙潭）1930-27-810.5%11.6%8.7%278-93-36.3%13.7%6.5%3693-89-010.8%17.4%9.0%4590-86-33.6%8.7%4.0%596-17-37.3%18.6%5.9%664-19-73.4%1.8%2.2%73208-16-07.6%10.3%9.7%8100432-32-713.8%10.5%11.1%9616-25-17.9%15.7%7.6%10108-88-313.0%18.9%11.1%1136099-44-25.6%16.4%12.9%121576-95-010.9%6.0%7.1%1325414-22-67.9%15.5%6.6%141551-16-26.1%16.1%7.5%15461-72-34.4%9.2%5.4%16928-97-216.0%5.0%5.8%17822-55-911.8%6.3%4.4%18110-43-04.2%11.0%6.4%193855-78-55.2%10.3%6.3%205911-04-068.1%7.1%2.4%2113475-82-68.9%13.2%10.7%2215869-93-97.9%12.4%10.3%23123-35-311.4%19.3%12.2%243777-69-39.8%16.9%9.4%2563169-61-96.1%12.1%10.6%26464-17-53.2%7.6%2.8%2762183-79-39.8%17.4%11.1%2813925-03-610.5%17.8%10.8%295989-27-58.5%18.1%10.2%3013466-78-912.4%12.6%7.4%3199-85-48.7%12.5%7.6%3299-86-517.0%14.8%10.6%3378-70-619.2%18.1%12.7%341072-83-99.5%8.5%8.5%3验证结果与汇总根据方法验证要求，牵头单位组织安捷伦科技有限公司、河南谱尼检测公司2家单位进行了方法验证，详见表4。仪器参数条件、前处理方法和各项性能指标均能满足方法要求。各参与验证单位使用牵头单位提供的茶叶样品，验证挥发性化合物种类、含量和精密度。每个样品称取2份进行实验，考察化合物种类及精密度是否达到20%内。2家参与单位的验证结果分别见表5-10。样品白龙潭安捷伦科技有限公司鉴定化合物数量为51个，谱尼检测公司鉴定化合物数量为67个，相同化合物数量为29个；样品车云山安捷伦科技有限公司鉴定化合物数量为51个，谱尼检测公司鉴定化合物数量为63个，相同化合物数量为32个；样品云雾山安捷伦科技有限公司鉴定化合物数量为50个，谱尼检测公司鉴定化合物数量为70个，相同化合物数量为26个；相同化合物作为标准附录1中参考化合物种类。各化合物精密度均率小于20%，满足分析的要求。表42家验证机构使用设备及耗材情况验证单位仪器色谱柱河南谱尼检测公司岛津GCMS-QP2020NXDB-624UI色谱柱（60m×0.25mm×1.4μm）安捷伦科技有限公司安捷伦8890-5977DB-624UI色谱柱（30m×0.25mm×1.4μm）由表4情况看出，2家验证机构所使用仪器、色谱柱有所不同，说明所建立方法的适用性、耐用性均可。表5白龙潭样品01风味挥发物质组成-安捷伦序号保留时间英文名称CAS号NIST匹配度（%）相对含量（%）1相对含量（%）2精密度15.3Furan,3-methyl-930-27-889.90.530.565.9725.92-Butanone78-93-386.20.570.538.1636.0EthylAcetate141-78-692.11.831.6510.3146.3Cyclopentene,1-methyl-693-89-086.20.330.369.2857.6Butanal,3-methyl-590-86-390.02.342.234.7367.9Butanal,2-methyl-96-17-388.76.926.388.0878.2Aceticacid64-19-795.16.656.246.3788.5Furan,2-ethyl-3208-16-092.21.211.127.9298.74-Methyl-2H-pyran1000432-32-782.80.050.059.00109.21-Penten-3-ol616-25-187.31.901.729.90119.5n-Propylacetate109-60-486.00.300.294.671211.2Toluene108-88-392.11.110.9219.021312.5Oxirane,2-(1,1-dimethylethyl)-3-ethyl-,cis-36099-44-286.60.860.7217.411412.82-Penten-1-ol,(Z)-1576-95-085.90.320.332.821513.2Furan,2-methoxy-25414-22-693.01.411.289.231613.3Aceticacid,butylester123-86-485.90.230.1918.751713.71H-Pyrrole,3-ethyl-1551-16-293.78.357.945.091813.8Hydantoin461-72-384.30.340.3110.021915.93-Hexen-1-ol,(E)-928-97-291.70.590.625.142016.61H-Imidazole-4-methanol822-55-988.71.001.066.052116.72-Heptanone110-43-085.50.290.2514.502218.02,3,4-Trimethylpyrrole3855-78-580.00.560.584.052318.1Nonane,3-methyl-5911-04-0686.90.260.260.002418.9Heptane,2,2,4,6,6-pentamethyl-13475-82-692.72.562.1318.422519.0Octane,3,5-dimethyl-15869-93-987.70.700.648.342619.1.beta.-Myrcene123-35-388.20.960.960.002719.4Furan,2-pentyl-3777-69-392.11.411.335.802819.9Pentanoicacid,2-methyl-,anhydride63169-61-989.50.090.0714.102920.2Bicyclo[2.2.1]hept-2-ene,1,7,7-trimethyl-464-17-583.90.790.879.303020.32,2,4,4-Tetramethyloctane62183-79-382.10.360.3212.543120.4Pyrazine,2-ethyl-6-methyl-13925-03-680.00.330.3610.573220.6D-Limonene5989-27-592.91.311.245.153320.7Bicyclo[3.1.1]hept-2-ene,3,6,6-trimethyl-4889-83-287.40.540.499.943421.23-Carene13466-78-992.20.850.832.553521.6.gamma.-Terpinene99-85-487.50.370.349.013622.0Butanedioicacid,dimethylester106-65-094.10.440.441.143722.61,3-Cyclohexadiene,1-methyl-4-(1-methylethyl)-99-86-588.60.530.497.353822.9Phenol,2-(aminomethyl)-932-30-981.11.721.653.933923.9Linalool78-70-690.30.490.5511.974024.2Ethanone,1-(1H-pyrrol-2-yl)-1072-83-980.70.470.483.604124.7Undecane,3-methyl-1002-43-380.50.490.501.074224.7Decane,3,8-dimethyl-17312-55-983.30.480.5818.374325.4Pentanedioicacid,dimethylester1119-40-090.71.381.259.244425.4PhenylethylAlcohol60-12-887.70.670.7611.644525.6Dodecane112-40-391.51.441.2216.714626.8(3R,6S)-2,2,6-Trimethyl…39028-58-585.60.490.4411.144728.5Undecane,4,6-dimethyl-17312-82-286.20.470.446.414828.5Undecane,3,5-dimethyl-17312-81-184.30.450.461.544928.84-Hexen-1-ol,5-methyl-2-(1-methylethenyl)-,(R)-498-16-880.70.480.5615.595035.3Naphthalene,1,2,4a,5,8,…523-47-780.50.400.4715.725145.2Caffeine58-08-291.37.487.322.24表6车云山样品02风味挥发物质组成-安捷伦序号保留时间英文名称CAS号NIST匹配度（%）相对含量（%）1相对含量（%）2精密度15.3Furan,3-methyl-930-27-887.40.560.543.6225.92-Butanone78-93-389.60.410.411.0236.0EthylAcetate141-78-690.21.941.940.0146.3Cyclopentene,1-methyl-693-89-086.60.340.324.3357.6Butanal,3-methyl-590-86-390.11.221.183.3167.9Butanal,2-methyl-96-17-387.93.313.280.8778.2Aceticacid64-19-795.56.906.960.9488.5Furan,2-ethyl-3208-16-091.61.141.094.4499.21-Penten-3-ol616-25-186.91.531.636.69109.32,3-Pentanedione600-14-688.70.790.823.351111.2Toluene108-88-392.00.630.688.101211.6Octane111-65-989.80.320.299.631312.5Oxirane,2-(1,1-dimethylethyl)-3-ethyl-,cis-36099-44-284.80.650.718.871413.2Furan,2-methoxy-25414-22-692.91.411.392.001513.3Aceticacid,butylester123-86-486.90.190.2735.871613.71H-Pyrrole,3-ethyl-1551-16-293.87.707.700.051713.83(2H)-Furanone,dihydro-2-methyl-3188-00-981.60.510.533.771815.2Benzene,1,3-dimethyl-108-38-386.70.150.165.791915.93-Hexen-1-ol,(E)-928-97-289.30.390.402.462016.61H-Imidazole-4-methanol106-65-489.60.810.855.252116.72-Heptanone110-43-081.50.210.204.602217.3Pyrazine,2,5-dimethyl-123-32-082.20.580.563.202318.02,3,4-Trimethylpyrrole3855-78-582.70.350.374.132418.0Nonane,3-methyl-5911-04-0688.90.260.247.182518.11-Pentanone,1-(2-furanyl)-3194-17-088.50.160.153.462618.9Heptane,2,2,4,6,6-pentamethyl-13475-82-691.62.142.203.072719.0Octane,3,5-dimethyl-15869-93-987.90.580.626.022819.1Bicyclo[3.1.1]heptane,6,6-dimethyl-2-methylene-,(1S)-18172-67-388.00.690.701.812919.4Furan,2-pentyl-3777-69-393.21.461.394.623020.2Bicyclo[2.2.1]hept-2-ene,1,7,7-trimethyl-464-17-583.40.780.754.123120.4Pyrazine,2-ethyl-6-methyl-13925-03-683.50.410.3514.043220.6D-Limonene5989-27-592.10.930.893.463320.7Bicyclo[3.1.1]hept-2-ene,3,6,6-trimethyl-4889-83-286.60.350.3015.563421.23-Carene13466-78-992.40.630.630.253521.6.gamma.-Terpinene99-85-484.00.280.259.383622.61,3-Cyclohexadiene,1-methyl-4-(1-methylethyl)-99-86-587.60.420.3418.723722.93-Hydroxy-4-methylbenzaldehyde57295-30-485.20.110.108.813822.9Phenol,2-(aminomethyl)-932-30-982.11.321.330.973923.01,2-Propanediol,1-phenyl-1855-09-080.41.000.7513.114023.9Linalool78-70-690.91.131.102.684124.2Ethanone,1-(1H-pyrrol-2-yl)-1072-83-982.60.580.602.414224.21,5,7-Octatrien-3-ol,3,7-dimethyl-29957-43-586.60.600.5214.124324.7p-Cresidine120-71-880.10.480.528.234425.4Benzenemethanol,.alpha.-methyl-98-85-187.20.580.580.934525.6Dodecane112-40-392.21.001.010.664626.74H-Pyran-4-one,2,3-dihydro-3,5-dihydroxy-6-methyl-28564-83-284.30.510.809.714728.5Undecane,4,6-dimethyl-17312-82-284.80.200.1511.214828.8Geraniol106-24-182.80.590.4612.314933.52-Cyclopenten-1-one,3-methyl-2-(2-pentenyl)-,(Z)-488-10-882.00.390.426.925033.7Cycloheptasiloxane,tetradecamethyl-107-50-683.90.410.4611.085145.2Caffeine58-08-289.56.506.450.82表7云雾山样品03风味挥发物质组成-安捷伦序号保留时间英文名称CAS号NIST匹配度（%）相对含量（%）1相对含量（%）2精密度15.3Furan,3-methyl-930-27-891.2605429.70.490.4725.8Silanol,trimethyl-1066-40-680.1172910.90.150.1335.92-Butanone78-93-390.3492687.80.350.3846.0EthylAcetate141-78-689.92247046.21.811.7556.3Cyclopentene,3-methyl-1120-62-380.2489873.00.330.3867.6Butanal,3-methyl-590-86-392.1957860.30.750.7477.9Butanal,2-methyl-96-17-387.82935325.52.332.2888.2Aceticacid64-19-795.77735729.55.686.0198.5Furan,2-ethyl-3208-16-092.9957104.10.790.74109.02-Pentanone107-87-989.979289.30.070.06119.2Propanoicacid,anhydride123-62-682.4901195.70.770.70129.5n-Propylacetate109-60-489.8236804.50.230.201310.9Acetoin513-86-091.0383256.30.340.301411.2Toluene108-88-391.0985627.90.840.771511.6Heptane,3-methyl-589-81-186.3242502.40.210.191613.2Furan,2-methoxy-25414-22-692.61509848.61.121.171713.3Aceticacid,butylester123-86-484.4237675.90.160.181813.71H-Pyrrole,3-ethyl-1551-16-293.010184979.27.957.911913.8Hydantoin461-72-387.2327773.90.410.352015.2Benzene,1,3-dimethyl-108-38-389.7258456.40.200.202115.93-Hexen-1-ol,(E)-928-97-291.9974825.30.730.762216.6Methylenecyclopropanecarboxylicacid62266-36-888.01535735.31.201.192318.02,3,4-Trimethylpyrrole3855-78-584.9759647.00.500.592418.0Undecane,6,6-dimethyl-17312-76-489.5343486.40.280.272518.9Heptane,2,2,4,6,6-pentamethyl-13475-82-694.83922334.02.893.052619.0Octane,3,5-dimethyl-15869-93-990.9777876.60.540.602719.1Bicyclo[3.1.1]heptane,6,6-dimethyl-2-methylene-,(1S)-18172-67-387.01197751.31.030.932819.4Furan,2-pentyl-3777-69-392.91220233.20.950.952920.21,3-Cyclohexadiene,1-methyl-4-(1-methylethyl)-99-86-583.2591473.00.730.663020.32,2,4,4-Tetramethyloctane62183-79-381.7481660.50.300.373120.6D-Limonene5989-27-592.91624487.51.251.263220.7Bicyclo[3.1.1]hept-2-ene,3,6,6-trimethyl-4889-83-283.8688288.70.500.533320.8.alpha.-Phellandrene99-83-281.2195639.30.230.193421.23-Carene13466-78-994.61153882.00.880.903521.6.gamma.-Terpinene99-85-486.4606017.80.400.473622.0Butanedioicacid,dimethylester106-65-092.178528.30.120.133722.62,4,6-Octatriene,2,6-dimethyl-673-84-787.3522122.20.410.413822.9Phenol,2-(aminomethyl)-932-30-981.21881399.21.541.463923.6Ethyl2-(5-methyl-5-vinyltetrahydrofuran-2-yl)propan-2-ylcarbonate1000373-80-384.21114546.90.740.874023.9Linalool78-70-690.91981304.11.611.544124.2Ethanone,1-(1H-pyrrol-2-yl)-1072-83-982.0587165.30.460.464224.7Decane,3,8-dimethyl-17312-55-988.9747305.30.490.584324.7p-Cresidine120-71-882.0754791.10.540.594425.4Pentanedioicacid,dimethylester1119-40-083.8379475.20.250.294525.4Benzenemethanol,.alpha.-methyl-98-85-190.6557133.90.500.434625.6Dodecane112-40-392.51401414.01.121.094726.8(3R,6S)-2,2,6-Trimethyl-6-vinyltetrahydro-2H-pyran-3-ol39028-58-584.8777717.20.610.604828.8Geraniol106-24-181.6689968.30.420.444935.2(1S,4S,4aS)-1-Isopropyl-4,7-dimethyl-1,2,3,4,4a,5-hexahydronaphthalene267665-20-381.6516163.40.550.465045.2Caffeine58-08-292.510780736.46.716.88表8白龙潭样品01风味挥发物质组成-谱尼序号保留时间英文名称CAS号NIST匹配度（%）相对含量（%）1相对含量（%）2精密度12.62Borane-methylsulfidecomplex13292-87-09333.8433.750.2723.20Aceticacid79-20-9960.860.842.3534.09Propanal,2-methyl-78-84-2975.315.290.3844.94Furan,3-methyl-930-27-8900.270.270.0055.362-Butyne-1,4-diol,diacetate1573-17-7810.380.372.6765.622-Butanone,4,4-dimethoxy-3-methyl-36075-03-3830.580.63.3975.78EthylAcetate141-78-69617.9317.581.9786.06Cyclopentene,1-methyl-693-89-0860.210.210.0097.49Butanal,3-methyl-590-86-3962.172.21.37107.78Butanal,2-methyl-96-17-3974.664.513.27118.47Furan,2-ethyl-3208-16-0960.80.867.23128.57Aceticacid64-19-7971.842.0812.24139.111-Penten-3-ol616-25-1971.631.757.10149.49n-Propylacetate109-60-4890.130.128.001510.43Propanoicacid,2-methyl-,2-methylbutylester2445-69-4880.410.395.001611.25Toluene108-88-3890.320.320.001711.293-Buten-2-one,3-methyl-814-78-8880.110.110.001811.69Hexane,2,4-dimethyl-589-43-5900.110.1316.671912.491-Pentanol71-41-0960.830.821.212012.772-Penten-1-ol,(Z)-1576-95-0950.310.310.002113.22Furan,2-methoxy-25414-22-6881.061.041.902213.36Aceticacid,butylester123-86-4900.190.190.002313.502,4-Dimethyl-1-heptene19549-87-2930.730.74.202413.751H-Pyrrole,1-ethyl-617-92-5913.133.081.612514.20Hexane,2,3,4-trimethyl-921-47-1830.30.339.522615.206-Octenal,7-methyl-3-methylene-55050-40-3830.080.080.002715.903-Hexen-1-ol,(E)-928-97-2950.630.641.572816.251-Hexanol111-27-3930.280.280.002916.621H-Imidazole-4-methanol822-55-9800.590.61.683016.772-Heptanone110-43-0920.190.25.133117.31Pyrazine,2,5-dimethyl-123-32-0910.160.156.453218.97cis-Geraniol106-25-2800.170.1911.113319.07Heptane,2,2,4,6,6-pentamethyl-13475-82-6971.181.125.223419.17Octane,3,5-dimethyl-15869-93-9910.170.166.063519.25Bicyclo[3.1.1]heptane,6,6-dimethyl-2-methylene-,(1S)-18172-67-3880.50.484.083619.43cis-2,6-Dimethyl-2,6-octadiene2492-22-0920.140.1613.333719.47Furan,2-pentyl-3777-69-3960.780.753.923819.69Decane,2,3,4-trimethyl-62238-15-7870.110.128.703919.951-Octyn-3-ol818-72-4800.330.342.994020.021-Octen-3-ol3391-86-4850.110.110.004120.255-Hepten-2-one,6-methyl-110-93-0930.160.156.454220.34Bicyclo[2.2.1]hept-2-ene,1,7,7-trimethyl-464-17-5820.220.29.524320.71D-Limonene5989-27-5930.460.472.154420.82trans-.beta.-Ocimene3779-61-1910.210.224.654520.90.alpha.-Phellandrene99-83-2840.080.080.004621.283-Carene13466-78-9900.460.472.154721.69.gamma.-Terpinene99-85-4900.130.147.414822.991H-Pyrrole-2-carboxaldehyde,1-ethyl-2167-14-8840.710.766.804923.05Benzylalcohol100-51-6930.390.382.605023.122-Furanmethanol,5-ethenyltetrahydro-.alpha.,.alpha.,5-trimethyl-,cis-5989-33-3890.410.395.005123.66Ethyl2-(5-methyl-5-vinyltetrahydrofuran-2-yl)propan-2-ylcarbonate1000373-84-3940.310.310.005223.97Linalool78-70-6960.860.860.005324.26Ethanone,1-(1H-pyrrol-2-yl)-1072-83-9950.360.345.715424.321,5,7-Octatrien-3-ol,3,7-dimethyl-29957-43-5930.460.452.205524.79p-Cresidine120-71-8860.190.25.135625.48PhenylethylAlcohol60-12-8960.560.535.505725.71Dodecane112-40-3960.640.614.805826.724H-Pyran-4-one,2,3-dihydro-3,5-dihydroxy-6-methyl-28564-83-2940.130.147.415926.91(3R,6S)-2,2,6-Trimethyl-6-vinyltetrahydro-2H-pyran-3-ol39028-58-5960.340.326.066028.00Butanoicacid,2-ethyl-,1,2,3-propanetriylester56554-54-2830.180.180.006128.90Geraniol106-24-1950.420.456.906230.08Benzofuran,2,3-dihydro-496-16-2850.110.128.706332.08Indole120-72-9800.050.0618.186433.39(E)-.beta.-Famesene18794-84-8890.090.090.006533.602-Cyclopenten-1-one,3-methyl-2-(2-pentenyl)-,(Z)-488-10-8910.180.195.416636.821,6,10-Dodecatrien-3-ol,3,7,11-trimethyl-,(E)-40716-66-3900.120.120.006745.29Caffeine58-08-2864.124.334.97表9车云山样品02风味挥发物质组成-谱尼序号保留时间英文名称CAS号NIST匹配度（%）相对含量（%）1相对含量（%）2精密度12.62Borane-methylsulfidecomplex13292-87-09324.9224.192.9723.17Aceticacid79-20-9962.472.594.7434.08Propanal,2-methyl-78-84-2974.143.983.9444.96Furan,3-methyl-930-27-8900.300.326.4555.362-Butyne-1,4-diol,diacetate1573-17-7810.440.432.3065.612-Butanone,4,4-dimethoxy-3-methyl-36075-03-3830.630.5611.7675.78EthylAcetate141-78-69627.3927.011.4086.07Cyclopentene,1-methyl-693-89-0860.220.220.0097.49Butanal,3-methyl-590-86-3961.331.32.28107.77Butanal,2-methyl-96-17-3972.962.795.91118.46Aceticacid64-19-7974.565.2614.26128.53Furan,2-ethyl-3208-16-0960.810.9313.79139.111-Penten-3-ol616-25-1971.551.560.64149.202,3-Pentanedione600-14-6950.270.257.691510.42Propanoicacid,2-methyl-,2-methylbutylester2445-69-4880.400.385.131611.24Toluene108-88-3890.290.283.511711.303-Buten-2-one,3-methyl-814-78-8880.150.1712.501811.69Hexane,2,4-dimethyl-589-43-5860.140.1613.331912.491-Pentanol71-41-0960.810.888.282012.772-Penten-1-ol,(Z)-1576-95-0950.300.313.282113.14Hexanal66-25-1830.070.0813.332213.22Furan,2-methoxy-25414-22-6881.161.279.052313.36Aceticacid,butylester123-86-4900.180.175.712413.502,4-Dimethyl-1-heptene19549-87-2930.740.731.362513.741H-Pyrrole,1-ethyl-617-92-5913.573.346.662614.19Hexane,2,3,4-trimethyl-921-47-1830.260.287.412715.903-Hexen-1-ol,(E)-928-97-2950.440.488.702816.251-Hexanol111-27-3930.310.336.252916.651H-Imidazole-4-methanol822-55-9800.590.636.563016.772-Heptanone110-43-0920.170.170.003117.32Pyrazine,2,5-dimethyl-123-32-0910.180.180.003218.96cis-Geraniol106-25-2800.170.166.063319.07Heptane,2,2,4,6,6-pentamethyl-13475-82-6971.111.037.483419.16Octane,3,5-dimethyl-15869-93-9910.180.180.003519.24Bicyclo[3.1.1]heptane,6,6-dimethyl-2-methylene-,(1S)-18172-67-3880.430.422.353619.47Furan,2-pentyl-3777-69-3961.041.040.003719.941-Octyn-3-ol818-72-4800.330.3711.433820.021-Octen-3-ol3391-86-4850.160.1811.763920.255-Hepten-2-one,6-methyl-110-93-0930.180.175.714020.33Bicyclo[2.2.1]hept-2-ene,1,7,7-trimethyl-464-17-5820.190.2110.004120.70D-Limonene5989-27-5930.40.424.884220.81trans-.beta.-Ocimene3779-61-1910.140.156.904321.273-Carene13466-78-9900.320.346.064421.69.gamma.-Terpinene99-85-4900.110.128.704522.981H-Pyrrole-2-carboxaldehyde,1-ethyl-2167-14-8840.700.8013.334623.05Benzylalcohol100-51-6930.620.586.674723.141-Octanol111-87-5880.450.462.204823.652-Furanmethanol,5-ethenyltetrahydro-.alpha.,.alpha.,5-trimethyl-,cis-5989-33-3890.360.372.744923.96Linalool78-70-6960.850.872.335024.26Ethanone,1-(1H-pyrrol-2-yl)-1072-83-9950.530.565.505124.321,5,7-Octatrien-3-ol,3,7-dimethyl-29957-43-5930.500.492.025224.79p-Cresidine120-71-8860.170.1911.115325.48PhenylethylAlcohol60-12-8960.480.448.705425.71Dodecane112-40-3960.450.474.355526.714H-Pyran-4-one,2,3-dihydro-3,5-dihydroxy-6-methyl-28564-83-2940.410.422.415626.90(3R,6S)-2,2,6-Trimethyl-6-vinyltetrahydro-2H-pyran-3-ol39028-58-5920.280.293.515728.00Butanoicacid,2-ethyl-,1,2,3-propanetriylester56554-54-2830.220.234.445828.90Geraniol106-24-1950.530.577.275931.77Hexanoicacid,3-hexenylester,(Z)-31501-11-8880.150.166.456033.39(E)-.beta.-Famesene18794-84-8890.130.128.006133.602-Cyclopenten-1-one,3-methyl-2-(2-pentenyl)-,(Z)-488-10-8910.220.2512.776236.821,6,10-Dodecatrien-3-ol,3,7,11-trimethyl-,(E)-40716-66-3900.170.185.716345.28Caffeine58-08-2864.984.960.40表10云雾山样品03风味挥发物质组成-谱尼序号保留时间英文名称CAS号NIST匹配度（%）相对含量（%）1相对含量（%）2精密度12.61Borane-methylsulfidecomplex13292-87-09323.9123.770.5923.16Aceticacid79-20-9961.381.324.4434.08Propanal,2-methyl-78-84-2973.663.670.2744.95Furan,3-methyl-930-27-8900.280.2511.3255.362-Butyne-1,4-diol,diacetate1573-17-7810.390.390.0065.622-Butanone,4,4-dimethoxy-3-methyl-36075-03-3830.520.5810.9175.78EthylAcetate141-78-69628.8327.793.6786.05Cyclopentene,1-methyl-693-89-0860.210.210.0097.49Butanal,3-methyl-590-86-3960.930.93.28107.77Butanal,2-methyl-96-17-3972.032.040.49118.48Furan,2-ethyl-3208-16-0960.480.5411.76128.53Aceticacid64-19-7973.994.4510.90139.111-Penten-3-ol616-25-1970.880.835.85149.202,3-Pentanedione600-14-6950.150.150.00159.49n-Propylacetate109-60-4910.150.1712.501610.42Propanoicacid,2-methyl-,2-methylbutylester2445-69-4880.460.4111.491711.24Toluene108-88-3890.30.293.391811.313-Buten-2-one,3-methyl-814-78-8880.080.080.001911.69Hexane,2,4-dimethyl-589-43-5860.150.166.452012.491-Pentanol71-41-0960.630.630.002112.762-Penten-1-ol,(Z)-1576-95-0950.170.166.062213.22Furan,2-methoxy-25414-22-6881.041.021.942313.36Aceticacid,butylester123-86-4900.200.195.132413.502,4-Dimethyl-1-heptene19549-87-2930.840.787.412513.741H-Pyrrole,1-ethyl-617-92-5913.253.322.132614.19Hexane,2,3,4-trimethyl-921-47-1830.290.2610.912715.206-Octenal,7-methyl-3-methylene-55050-40-3830.210.204.882815.23Benzene,1,3-dimethyl-108-38-3820.060.060.002915.903-Hexen-1-ol,(E)-928-97-2950.890.901.123016.251-Hexanol111-27-3930.390.382.603116.621H-Imidazole-4-methanol822-55-9800.890.901.123216.772-Heptanone110-43-0920.130.130.003317.31Pyrazine,2,5-dimethyl-123-32-0910.130.147.413418.97cis-Geraniol106-25-2800.200.200.003519.07Heptane,2,2,4,6,6-pentamethyl-13475-82-6;97971.051.040.963619.17Octane,3,5-dimethyl-15869-93-9910.180.175.713719.25Bicyclo[3.1.1]heptane,6,6-dimethyl-2-methylene-,(1S)-18172-67-3880.610.621.633819.41cis-2,6-Dimethyl-2,6-octa