《信陽(yáng)毛尖茶中風(fēng)味揮發(fā)物質(zhì)的測(cè)定》團(tuán)體標(biāo)準(zhǔn)編制說明

1、信陽(yáng)毛尖茶中風(fēng)味揮發(fā)物質(zhì)測(cè)定 氣相色譜質(zhì)譜法團(tuán)體標(biāo)準(zhǔn)編制說明1 工作簡(jiǎn)況1.1任務(wù)來源 本項(xiàng)目是根據(jù)河南省食品工業(yè)協(xié)會(huì)2021年團(tuán)體標(biāo)準(zhǔn)項(xiàng)目征集計(jì)劃文件（豫食協(xié)202103號(hào)），協(xié)會(huì)標(biāo)準(zhǔn)專業(yè)委員會(huì)進(jìn)行了立項(xiàng)評(píng)審，符合立項(xiàng)條件，批準(zhǔn)立項(xiàng)。項(xiàng)目批準(zhǔn)立項(xiàng)文件為：豫食協(xié)202104號(hào)，項(xiàng)目名稱為：信陽(yáng)毛尖茶風(fēng)味揮發(fā)物質(zhì)的測(cè)定。1.2主要工作過程標(biāo)準(zhǔn)制定計(jì)劃下達(dá)后，在河南省食品工業(yè)協(xié)會(huì)標(biāo)準(zhǔn)專業(yè)委員會(huì)的領(lǐng)導(dǎo)下，主要起草單位認(rèn)真落實(shí)和實(shí)施計(jì)劃，牽頭成立了標(biāo)準(zhǔn)起草工作組(以下簡(jiǎn)稱“工作組”)。工作組在調(diào)查、收集、研究有關(guān)標(biāo)準(zhǔn)資料及分析、研究信陽(yáng)毛尖茶風(fēng)味揮發(fā)物質(zhì)測(cè)定的基礎(chǔ)上制定了檢測(cè)技術(shù)路線。研制過程中，結(jié)合

2、日常文獻(xiàn)收集、摸底調(diào)研等前期工作基礎(chǔ)，對(duì)相關(guān)內(nèi)容進(jìn)行驗(yàn)證、完善，建立了頂空氣相色譜質(zhì)譜測(cè)定方法。期間多次易稿修改，最終建立方法并組織2家單位進(jìn)行實(shí)驗(yàn)室間驗(yàn)證，于2022年4月底完成了標(biāo)準(zhǔn)征求意見稿及其編制說明。2標(biāo)準(zhǔn)編制原則和主要內(nèi)容的論據(jù)2.1標(biāo)準(zhǔn)編制原則本文件的編制以技術(shù)的先進(jìn)性、標(biāo)準(zhǔn)的適用性、統(tǒng)一性、協(xié)調(diào)性為原則。標(biāo)準(zhǔn)的結(jié)構(gòu)及編寫方法按GB/T 1.1-2020標(biāo)準(zhǔn)化工作導(dǎo)則第1部分：標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則。2.2 標(biāo)準(zhǔn)主要技術(shù)內(nèi)容方法規(guī)定了信陽(yáng)毛尖茶風(fēng)味揮發(fā)物質(zhì)測(cè)定的頂空氣相色譜質(zhì)譜測(cè)定方法。本方法適用于信陽(yáng)毛尖茶風(fēng)味揮發(fā)物質(zhì)的測(cè)定。2.3 各項(xiàng)技術(shù)指標(biāo)確立的原則和論據(jù)（1）檢測(cè)技

3、術(shù)路線信陽(yáng)毛尖茶風(fēng)味揮發(fā)物質(zhì)測(cè)定方法比較多，經(jīng)查閱文獻(xiàn)，發(fā)現(xiàn)測(cè)定方法有熱脫附氣相色譜質(zhì)譜法、液相色譜串接質(zhì)譜法、氣相色譜串接質(zhì)譜法、頂空氣相色譜高分辨質(zhì)譜法等。其中，液相色譜串接質(zhì)譜法測(cè)定低分子量香精種類少，靈敏度不足；熱脫附氣相色譜質(zhì)譜法具有高靈敏度、快速、選擇性好的特點(diǎn)，但是重現(xiàn)性較差，對(duì)吸附材料有特殊要求，方法普及性差；氣相色譜串接質(zhì)譜法對(duì)特定種類的香精具有高靈敏度和高重現(xiàn)性，但是需要對(duì)茶葉進(jìn)行前處理，測(cè)定的化合物種類必須提前設(shè)定好方法。頂空氣相色譜高分辨質(zhì)譜法檢測(cè)靈敏度高，但是沒有公開公認(rèn)的高分辨質(zhì)譜庫(kù)。采用頂空氣相色譜質(zhì)譜檢測(cè),能夠?qū)Σ煌N類綠茶進(jìn)行測(cè)定，化合物可使用NIST庫(kù)進(jìn)行識(shí)

4、別定性，普及性強(qiáng)，操作簡(jiǎn)單。最終技術(shù)路線為：茶葉經(jīng)粉碎過篩，采用頂空氣相色譜質(zhì)譜檢測(cè)，使用NIST庫(kù)進(jìn)行識(shí)別定性，峰面積歸一化法定量。茶葉樣品處理綠茶按照GB/T 18795-2012制樣，稱取待測(cè)綠茶2g于20mL頂空瓶中，密封，待測(cè)。色譜柱的選擇本研究測(cè)定的是揮發(fā)性化合物，因此沒有采用液體進(jìn)樣的色譜柱（通常膜厚0.25m），采用揮發(fā)性化合物測(cè)定色譜柱DB-624UI 色譜柱（30 m0.25 mm1.4 m）（膜厚1.4m）對(duì)揮發(fā)性化合物分離效果好。升溫程序優(yōu)化研究比較了兩種升溫程序，升溫程序A，40 保持3 min，以5 /min升至260 ；升溫程序B色譜柱初始溫度40，保持1min，

5、20/min到180，然后5/min到260保持5min；兩種綠茶（代號(hào)p、x）在不同升溫程序色譜圖，見圖1、2。圖1 升溫程序A條件下綠茶p和綠茶x總離子流圖圖2 升溫程序A條件下綠茶p和綠茶x總離子流圖升溫程序A升溫速度較慢，檢測(cè)時(shí)間長(zhǎng)，化合物分離效果好。升溫程序B速度快，節(jié)省檢測(cè)時(shí)間，但化合物分離效果差，尤其是2min20min段化合物不能有效分離?？紤]到定性是根據(jù)峰質(zhì)譜圖匹配，峰分不開會(huì)嚴(yán)重影響定性準(zhǔn)確度，因此采用升溫程序A。頂空溫度選擇加熱溫度是頂空進(jìn)樣重要的參數(shù)，改變加熱溫度能夠影響頂空氣中揮發(fā)物的種類和含量。研究選用了兩種綠茶（代號(hào)p、x），在平衡溫度50min條件下，進(jìn)行溫度單

6、因素實(shí)驗(yàn)，加熱溫度分別為：60、80、100、120、140?？傠x子流圖見圖3。圖3 不同頂空加熱溫度下綠茶p和綠茶x總離子流圖從圖3可以看出，隨加熱溫度提高，出峰數(shù)量整體呈現(xiàn)增加的趨勢(shì)。但在較高溫度下（140）出峰數(shù)量減少，減少的化合物主要在10min-20min，屬于高沸點(diǎn)化合物?？赡艿脑蚴沁@些化合物在高溫下參與化學(xué)反應(yīng)，導(dǎo)致檢測(cè)化合物數(shù)量較少。不同頂空加熱溫度下總離子流圖積分提取化合物，積分時(shí)忽略峰面積最大峰面積5%的化合物，化合物提取數(shù)量見表2。表2化合物提取數(shù)量溫度，綠茶x化合物數(shù)量，個(gè)綠茶p化合物數(shù)量，個(gè)6043802021100343612060601405148從表2中可以看

7、出，溫度120化合物數(shù)量最多，為60個(gè)。因此本部分選擇最佳頂空溫度為120。平衡時(shí)間的選擇考察了頂空溫度為120，綠茶x其中3個(gè)不同保留時(shí)間的化合物（保留時(shí)間3.3min、8.2min、12.1min），在30min、40min、50min、60min、70min的峰面積。將最大峰面積設(shè)為1，面積面積歸一化計(jì)算3個(gè)化合物在不同溫度下的峰面積。結(jié)果見圖4圖4 不同頂空平衡時(shí)間對(duì)化合物峰面積響應(yīng)影響從圖4可以看出，隨著平衡時(shí)間延長(zhǎng)，化合物響應(yīng)逐漸變大，在50min以后，化合物響應(yīng)不再顯著升高?？紤]到過長(zhǎng)加熱時(shí)間浪費(fèi)能源，延長(zhǎng)檢測(cè)時(shí)間。因此，選擇平衡時(shí)間50min。方法學(xué)考察樣品來源：信陽(yáng)毛尖茶3批

8、次，分別產(chǎn)自信陽(yáng)云霧山、車云山、白龍?zhí)??；衔锓N類：3批次茶葉中鑒定出匹配度80%化合物數(shù)量34種，精密度均在20%以內(nèi)，詳見表3。表3 茶葉中揮發(fā)性化合物種類及精密度（RSD）序號(hào)cas號(hào)信陽(yáng)毛尖（云霧山）信陽(yáng)毛尖（車云山）信陽(yáng)毛尖（白龍?zhí)叮?930-27-810.5%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

9、%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.

10、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%1

11、8.1%12.7%341072-83-99.5%8.5%8.5%3 驗(yàn)證結(jié)果與匯總根據(jù)方法驗(yàn)證要求，牽頭單位組織安捷倫科技有限公司、河南譜尼檢測(cè)公司2家單位進(jìn)行了方法驗(yàn)證，詳見表4。儀器參數(shù)條件、前處理方法和各項(xiàng)性能指標(biāo)均能滿足方法要求。各參與驗(yàn)證單位使用牽頭單位提供的茶葉樣品，驗(yàn)證揮發(fā)性化合物種類、含量和精密度。每個(gè)樣品稱取2份進(jìn)行實(shí)驗(yàn)，考察化合物種類及精密度是否達(dá)到20%內(nèi)。2家參與單位的驗(yàn)證結(jié)果分別見表5-10。樣品白龍?zhí)栋步輦惪萍加邢薰捐b定化合物數(shù)量為51個(gè)，譜尼檢測(cè)公司鑒定化合物數(shù)量為67個(gè)，相同化合物數(shù)量為29個(gè)；樣品車云山安捷倫科技有限公司鑒定化合物數(shù)量為51個(gè)，譜尼檢測(cè)公司鑒

12、定化合物數(shù)量為63個(gè)，相同化合物數(shù)量為32個(gè)；樣品云霧山安捷倫科技有限公司鑒定化合物數(shù)量為50個(gè)，譜尼檢測(cè)公司鑒定化合物數(shù)量為70個(gè)，相同化合物數(shù)量為26個(gè)；相同化合物作為標(biāo)準(zhǔn)附錄1中參考化合物種類。各化合物精密度均率小于20%，滿足分析的要求。表4 2家驗(yàn)證機(jī)構(gòu)使用設(shè)備及耗材情況驗(yàn)證單位儀器色譜柱河南譜尼檢測(cè)公司島津 GCMS-QP2020 NXDB-624UI 色譜柱（60 m0.25 mm1.4 m）安捷倫科技有限公司安捷倫8890-5977DB-624UI 色譜柱（30 m0.25 mm1.4 m）由表4情況看出，2家驗(yàn)證機(jī)構(gòu)所使用儀器、色譜柱有所不同，說明所建立方法的適用性、耐用性均

13、可。表5 白龍?zhí)稑悠?1風(fēng)味揮發(fā)物質(zhì)組成-安捷倫序號(hào)保留時(shí)間英文名稱CAS號(hào)NIST匹配度（%）相對(duì)含量（%）1相對(duì)含量（%）2精密度15.3Furan, 3-methyl-930-27-889.90.530.565.9725.92-Butanone78-93-386.20.570.538.1636.0Ethyl Acetate141-78-692.11.831.6510.3146.3Cyclopentene, 1-methyl-693-89-086.20.330.369.2857.6Butanal, 3-methyl-590-86-390.02.342.234.7367.9Butanal,

14、2-methyl-96-17-388.76.926.388.0878.2Acetic acid64-19-795.16.656.246.3788.5Furan, 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-Propyl acetate109-60-486.00.300.294.671211.2Toluene108-88-392.11.110.9219.021312.5Oxiran

15、e, 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-25414-22-693.01.411.289.231613.3Acetic acid, butyl ester123-86-485.90.230.1918.751713.71H-Pyrrole, 3-ethyl-1551-16-293.78.357.945.091813.8Hydantoin461-72-384.30.

16、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-13475-8

17、2-692.72.562.1318.422519.0Octane, 3,5-dimethyl-15869-93-987.70.700.648.342619.1.beta.-Myrcene123-35-388.20.960.960.002719.4Furan, 2-pentyl-3777-69-392.11.411.335.802819.9Pentanoic acid, 2-methyl-, anhydride63169-61-989.50.090.0714.102920.2Bicyclo2.2.1hept-2-ene, 1,7,7-trimethyl-464-17-583.90.790.879

18、.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-Limonene5989-27-592.91.311.245.153320.7Bicyclo3.1.1hept-2-ene, 3,6,6-trimethyl-4889-83-287.40.540.499.943421.23-Carene13466-78-992.20.850.832.553521.6.gamma.-Terpinene99-8

19、5-487.50.370.349.013622.0Butanedioic acid, dimethyl ester106-65-094.10.440.441.143722.61,3-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)-1072-83-980.70.4

20、70.483.604124.7Undecane, 3-methyl-1002-43-380.50.490.501.074224.7Decane, 3,8-dimethyl-17312-55-983.30.480.5818.374325.4Pentanedioic acid, dimethyl ester1119-40-090.71.381.259.244425.4Phenylethyl Alcohol60-12-887.70.670.7611.644525.6Dodecane112-40-391.51.441.2216.714626.8(3R,6S)-2,2,6-Trimethyl39028-

21、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

22、.24表6 車云山樣品02風(fēng)味揮發(fā)物質(zhì)組成-安捷倫序號(hào)保留時(shí)間英文名稱CAS號(hào)NIST匹配度（%）相對(duì)含量（%）1相對(duì)含量（%）2精密度15.3Furan, 3-methyl-930-27-887.40.560.543.6225.92-Butanone78-93-389.60.410.411.0236.0Ethyl Acetate141-78-690.21.941.940.0146.3Cyclopentene, 1-methyl-693-89-086.60.340.324.3357.6Butanal, 3-methyl-590-86-390.11.221.183.3167.9Butanal,

23、2-methyl-96-17-387.93.313.280.8778.2Acetic acid64-19-795.56.906.960.9488.5Furan, 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-dimet

24、hylethyl)-3-ethyl-, cis-36099-44-284.80.650.718.871413.2Furan, 2-methoxy-25414-22-692.91.411.392.001513.3Acetic acid, butyl ester123-86-486.90.190.2735.871613.71H-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

25、-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-

26、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-15869-93-987.90.580.626.022819.1Bicyclo3.1.1heptane, 6,6-dimethyl-2-methylene-, (1S)-18172-67-388.00.690.701.812919.4Furan, 2-pentyl-3

27、777-69-393.21.461.394.623020.2Bicyclo2.2.1hept-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-Limonene5989-27-592.10.930.893.463320.7Bicyclo3.1.1hept-2-ene, 3,6,6-trimethyl-4889-83-286.60.350.3015.563421.23-Carene13466-78-992.40.630

28、.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-1855-09-080.41.000.751

29、3.114023.9Linalool78-70-690.91.131.102.684124.2Ethanone, 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-98-85-187.20.580.580.934525.6Dodecane112-40-392.21.0

30、01.010.664626.74H-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, tetrad

31、ecamethyl-107-50-683.90.410.4611.085145.2Caffeine58-08-289.56.506.450.82表7 云霧山樣品03風(fēng)味揮發(fā)物質(zhì)組成-安捷倫序號(hào)保留時(shí)間英文名稱CAS號(hào)NIST匹配度（%）相對(duì)含量（%）1相對(duì)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-Butanone78-93-390.3492687.80.350.3846.0Ethyl Acetate141-7

32、8-689.92247046.21.811.7556.3Cyclopentene, 3-methyl-1120-62-380.2489873.00.330.3867.6Butanal, 3-methyl-590-86-392.1957860.30.750.7477.9Butanal, 2-methyl-96-17-387.82935325.52.332.2888.2Acetic acid64-19-795.77735729.55.686.0198.5Furan, 2-ethyl-3208-16-092.9957104.10.790.74109.02-Pentanone107-87-989.97

33、9289.30.070.06119.2Propanoic acid, anhydride123-62-682.4901195.70.770.70129.5n-Propyl acetate109-60-489.8236804.50.230.201310.9Acetoin513-86-091.0383256.30.340.301411.2Toluene108-88-391.0985627.90.840.771511.6Heptane, 3-methyl-589-81-186.3242502.40.210.191613.2Furan, 2-methoxy-25414-22-692.61509848.

34、61.121.171713.3Acetic acid, butyl ester123-86-484.4237675.90.160.181813.71H-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)-928-97-291.9974825.30.730.762216.6Methylenecyclopropa

35、necarboxylic acid62266-36-888.01535735.31.201.192318.02,3,4-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-15869-93-990.9777876.60.540.602719.1Bicyc

36、lo3.1.1heptane, 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.

37、91624487.51.251.263220.7Bicyclo3.1.1hept-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.-Terpinene99-85-486.4606017.80.400.473622.0Butanedioic acid, dimethyl ester106-65-092.178528.30.

38、120.133722.62,4,6-Octatriene, 2,6-dimethyl-673-84-787.3522122.20.410.413822.9Phenol, 2-(aminomethyl)-932-30-981.21881399.21.541.463923.6Ethyl 2-(5-methyl-5-vinyltetrahydrofuran-2-yl)propan-2-yl carbonate1000373-80-384.21114546.90.740.874023.9Linalool78-70-690.91981304.11.611.544124.2Ethanone, 1-(1H-

39、pyrrol-2-yl)-1072-83-982.0587165.30.460.464224.7Decane, 3,8-dimethyl-17312-55-988.9747305.30.490.584324.7p-Cresidine120-71-882.0754791.10.540.594425.4Pentanedioic acid, dimethyl ester1119-40-083.8379475.20.250.294525.4Benzenemethanol, .alpha.-methyl-98-85-190.6557133.90.500.434625.6Dodecane112-40-39

40、2.51401414.01.121.094726.8(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

41、.88表8 白龍?zhí)稑悠?1風(fēng)味揮發(fā)物質(zhì)組成-譜尼序號(hào)保留時(shí)間英文名稱CAS號(hào)NIST匹配度（%）相對(duì)含量（%）1相對(duì)含量（%）2精密度12.62Borane-methyl sulfide complex13292 - 87 - 09333.8433.750.2723.20Acetic acid79 - 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, diacetat

42、e1573 - 17 - 7810.380.372.6765.622-Butanone, 4,4-dimethoxy-3-methyl-36075 - 03 - 3830.580.63.3975.78Ethyl Acetate141 - 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 - 3974.664.513.27118.47Fu

43、ran, 2-ethyl-3208-16-0960.80.867.23128.57Acetic acid64 - 19 - 7971.842.0812.24139.111-Penten-3-ol616-25-1971.631.757.10149.49n-Propyl acetate109 - 60 - 4890.130.128.001510.43Propanoic acid, 2-methyl-, 2-methylbutyl ester2445 - 69 - 4880.410.395.001611.25Toluene108 - 88 - 3890.320.320.001711.293-Bute

44、n-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 - 6881.061.041.902213.36Acetic acid, butyl ester123 - 86 - 4900.190.190

45、.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-Hexan

46、ol111 - 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 - 6971.181.125.223419.1

47、7Octane, 3,5-dimethyl-15869 - 93 - 9910.170.166.063519.25Bicyclo3.1.1heptane, 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

48、.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 - 0930.160.156.454220.34Bicyclo2.2.1hept-2-ene, 1,7,7-trimethyl-464 - 17 - 5820.220.29.524320.71D-Limonene5989 - 27 - 5930.460.472.154420.82trans-.beta.-Ocim

49、ene3779 - 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 - 8840.710.766.804923.05Benzyl alcohol100 - 51 - 6930.390.382.605023.122-

50、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 - 9950.360.345.71542

51、4.321,5,7-Octatrien-3-ol, 3,7-dimethyl-29957 - 43 - 5930.460.452.205524.79p-Cresidine120 - 71 - 8860.190.25.135625.48Phenylethyl Alcohol60-12-8960.560.535.505725.71Dodecane112 - 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

52、,2,6-Trimethyl-6-vinyltetrahydro-2H-pyran-3-ol39028 - 58 - 5960.340.326.066028.00Butanoic acid, 2-ethyl-, 1,2,3-propanetriyl ester56554 - 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

53、.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 車云山樣品02風(fēng)味揮發(fā)物質(zhì)組成-譜尼序號(hào)保留時(shí)間英文名稱CAS號(hào)NIST匹配度（%）相對(duì)

54、含量（%）1相對(duì)含量（%）2精密度12.62 Borane-methylsulfidecomplex13292-87-09324.9224.192.97 23.17 Aceticacid79-20-9962.472.594.74 34.08 Propanal,2-methyl-78-84-2974.143.983.94 44.96 Furan,3-methyl-930-27-8900.300.326.45 55.36 2-Butyne-1,4-diol,diacetate1573-17-7810.440.432.30 65.61 2-Butanone,4,4-dimethoxy-3-methy

55、l-36075-03-3830.630.5611.76 75.78 EthylAcetate141-78-69627.3927.011.40 86.07 Cyclopentene,1-methyl-693-89-0860.220.220.00 97.49 Butanal,3-methyl-590-86-3961.331.32.28 107.77 Butanal,2-methyl-96-17-3972.962.795.91 118.46 Aceticacid64-19-7974.565.2614.26 128.53 Furan,2-ethyl-3208-16-0960.810.9313.79 1

56、39.11 1-Penten-3-ol616-25-1971.551.560.64 149.20 2,3-Pentanedione600-14-6950.270.257.69 1510.42 Propanoic acid, 2-methyl-, 2-methylbutyl ester2445 - 69 - 4880.400.385.13 1611.24 Toluene108-88-3890.290.283.51 1711.30 3-Buten-2-one,3-methyl-814-78-8880.150.1712.50 1811.69Hexane,2,4-dimethyl-589-43-586

57、0.140.1613.33 1912.49 1-Pentanol71-41-0960.810.888.28 2012.77 2-Penten-1-ol,(Z)-1576-95-0950.300.313.28 2113.14 Hexanal66-25-1830.070.0813.33 2213.22 Furan,2-methoxy-25414-22-6881.161.279.05 2313.36 Aceticacid,butylester123-86-4900.180.175.71 2413.50 2,4-Dimethyl-1-heptene19549-87-2930.740.731.36 25

58、13.74 1H-Pyrrole,1-ethyl-617-92-5913.573.346.66 2614.19 Hexane,2,3,4-trimethyl-921-47-1830.260.287.41 2715.90 3-Hexen-1-ol,(E)-928-97-2950.440.488.70 2816.25 1-Hexanol111-27-3930.310.336.25 2916.65 1H-Imidazole-4-methanol822-55-9800.590.636.56 3016.77 2-Heptanone110-43-0920.170.170.00 3117.32 Pyrazi

59、ne,2,5-dimethyl-123-32-0910.180.180.00 3218.96 cis-Geraniol106-25-2800.170.166.06 3319.07 Heptane,2,2,4,6,6-pentamethyl-13475-82-6971.111.037.48 3419.16 Octane,3,5-dimethyl-15869-93-9910.180.180.00 3519.24 Bicyclo3.1.1heptane,6,6-dimethyl-2-methylene-,(1S)-18172-67-3880.430.422.35 3619.47 Furan,2-pe

60、ntyl-3777-69-3961.041.040.00 3719.94 1-Octyn-3-ol818-72-4800.330.3711.43 3820.02 1-Octen-3-ol3391-86-4850.160.1811.76 3920.25 5-Hepten-2-one,6-methyl-110-93-0930.180.175.71 4020.33 Bicyclo2.2.1hept-2-ene,1,7,7-trimethyl-464-17-5820.190.2110.00 4120.70 D-Limonene5989-27-5930.40.424.88 4220.81 trans-.