CN107543882A - A kind of method for determining liquor flavor component synthesis molecular weight - Google Patents
A kind of method for determining liquor flavor component synthesis molecular weight Download PDFInfo
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- CN107543882A CN107543882A CN201710735483.3A CN201710735483A CN107543882A CN 107543882 A CN107543882 A CN 107543882A CN 201710735483 A CN201710735483 A CN 201710735483A CN 107543882 A CN107543882 A CN 107543882A
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- volatile
- molecular weight
- ethyl
- white spirit
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000000796 flavoring agent Substances 0.000 title claims abstract description 26
- 235000019634 flavors Nutrition 0.000 title claims abstract description 26
- 230000015572 biosynthetic process Effects 0.000 title abstract 3
- 238000003786 synthesis reaction Methods 0.000 title abstract 3
- 239000000126 substance Substances 0.000 claims abstract description 38
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 11
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 13
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- SHZIWNPUGXLXDT-UHFFFAOYSA-N ethyl hexanoate Chemical compound CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 claims description 10
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 10
- QPRQEDXDYOZYLA-UHFFFAOYSA-N 2-methylbutan-1-ol Chemical compound CCC(C)CO QPRQEDXDYOZYLA-UHFFFAOYSA-N 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- WWZKQHOCKIZLMA-UHFFFAOYSA-N Caprylic acid Natural products CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000004817 gas chromatography Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 8
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 claims description 6
- YGHRJJRRZDOVPD-UHFFFAOYSA-N 3-methylbutanal Chemical compound CC(C)CC=O YGHRJJRRZDOVPD-UHFFFAOYSA-N 0.000 claims description 6
- ROWKJAVDOGWPAT-UHFFFAOYSA-N Acetoin Chemical compound CC(O)C(C)=O ROWKJAVDOGWPAT-UHFFFAOYSA-N 0.000 claims description 6
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 6
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 6
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 6
- 239000004386 Erythritol Substances 0.000 claims description 6
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 claims description 6
- 229930195725 Mannitol Natural products 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 6
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 claims description 6
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 6
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 6
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 claims description 6
- 235000019414 erythritol Nutrition 0.000 claims description 6
- 229940009714 erythritol Drugs 0.000 claims description 6
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 claims description 6
- RGXWDWUGBIJHDO-UHFFFAOYSA-N ethyl decanoate Chemical compound CCCCCCCCCC(=O)OCC RGXWDWUGBIJHDO-UHFFFAOYSA-N 0.000 claims description 6
- TVQGDYNRXLTQAP-UHFFFAOYSA-N ethyl heptanoate Chemical compound CCCCCCC(=O)OCC TVQGDYNRXLTQAP-UHFFFAOYSA-N 0.000 claims description 6
- XIRNKXNNONJFQO-UHFFFAOYSA-N ethyl hexadecanoate Chemical compound CCCCCCCCCCCCCCCC(=O)OCC XIRNKXNNONJFQO-UHFFFAOYSA-N 0.000 claims description 6
- MMKRHZKQPFCLLS-UHFFFAOYSA-N ethyl myristate Chemical compound CCCCCCCCCCCCCC(=O)OCC MMKRHZKQPFCLLS-UHFFFAOYSA-N 0.000 claims description 6
- YYZUSRORWSJGET-UHFFFAOYSA-N ethyl octanoate Chemical compound CCCCCCCC(=O)OCC YYZUSRORWSJGET-UHFFFAOYSA-N 0.000 claims description 6
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 6
- FBPFZTCFMRRESA-GUCUJZIJSA-N galactitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-GUCUJZIJSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 claims description 6
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000845 maltitol Substances 0.000 claims description 6
- VQHSOMBJVWLPSR-WUJBLJFYSA-N maltitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-WUJBLJFYSA-N 0.000 claims description 6
- 235000010449 maltitol Nutrition 0.000 claims description 6
- 229940035436 maltitol Drugs 0.000 claims description 6
- 239000000594 mannitol Substances 0.000 claims description 6
- 235000010355 mannitol Nutrition 0.000 claims description 6
- JYVLIDXNZAXMDK-UHFFFAOYSA-N pentan-2-ol Chemical compound CCCC(C)O JYVLIDXNZAXMDK-UHFFFAOYSA-N 0.000 claims description 6
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000000600 sorbitol Substances 0.000 claims description 6
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000811 xylitol Substances 0.000 claims description 6
- 235000010447 xylitol Nutrition 0.000 claims description 6
- 229960002675 xylitol Drugs 0.000 claims description 6
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 6
- HEBKCHPVOIAQTA-QWWZWVQMSA-N D-arabinitol Chemical compound OC[C@@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-QWWZWVQMSA-N 0.000 claims description 4
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 4
- OWBTYPJTUOEWEK-UHFFFAOYSA-N butane-2,3-diol Chemical compound CC(O)C(C)O OWBTYPJTUOEWEK-UHFFFAOYSA-N 0.000 claims description 4
- 238000004587 chromatography analysis Methods 0.000 claims description 4
- 229960005150 glycerol Drugs 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- JLIDRDJNLAWIKT-UHFFFAOYSA-N 1,2-dimethyl-3h-benzo[e]indole Chemical compound C1=CC=CC2=C(C(=C(C)N3)C)C3=CC=C21 JLIDRDJNLAWIKT-UHFFFAOYSA-N 0.000 claims description 3
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 claims description 3
- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 claims description 3
- GWYFCOCPABKNJV-UHFFFAOYSA-M 3-Methylbutanoic acid Natural products CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 claims description 3
- XVSZRAWFCDHCBP-UHFFFAOYSA-N 3-methylbutyl hexanoate Chemical compound CCCCCC(=O)OCCC(C)C XVSZRAWFCDHCBP-UHFFFAOYSA-N 0.000 claims description 3
- AWQSAIIDOMEEOD-UHFFFAOYSA-N 5,5-Dimethyl-4-(3-oxobutyl)dihydro-2(3H)-furanone Chemical compound CC(=O)CCC1CC(=O)OC1(C)C AWQSAIIDOMEEOD-UHFFFAOYSA-N 0.000 claims description 3
- RPRPDTXKGSIXMD-UHFFFAOYSA-N Caproic acid n-butyl ester Natural products CCCCCC(=O)OCCCC RPRPDTXKGSIXMD-UHFFFAOYSA-N 0.000 claims description 3
- LVGKNOAMLMIIKO-UHFFFAOYSA-N Elaidinsaeure-aethylester Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC LVGKNOAMLMIIKO-UHFFFAOYSA-N 0.000 claims description 3
- ICMAFTSLXCXHRK-UHFFFAOYSA-N Ethyl pentanoate Chemical compound CCCCC(=O)OCC ICMAFTSLXCXHRK-UHFFFAOYSA-N 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 3
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 3
- 150000001241 acetals Chemical class 0.000 claims description 3
- DULCUDSUACXJJC-UHFFFAOYSA-N benzeneacetic acid ethyl ester Natural products CCOC(=O)CC1=CC=CC=C1 DULCUDSUACXJJC-UHFFFAOYSA-N 0.000 claims description 3
- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 claims description 3
- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 claims description 3
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims description 3
- 229940116333 ethyl lactate Drugs 0.000 claims description 3
- FMMOOAYVCKXGMF-MURFETPASA-N ethyl linoleate Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(=O)OCC FMMOOAYVCKXGMF-MURFETPASA-N 0.000 claims description 3
- 229940031016 ethyl linoleate Drugs 0.000 claims description 3
- LVGKNOAMLMIIKO-QXMHVHEDSA-N ethyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC LVGKNOAMLMIIKO-QXMHVHEDSA-N 0.000 claims description 3
- 229940093471 ethyl oleate Drugs 0.000 claims description 3
- 229940067592 ethyl palmitate Drugs 0.000 claims description 3
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 229940117955 isoamyl acetate Drugs 0.000 claims description 3
- FMMOOAYVCKXGMF-UHFFFAOYSA-N linoleic acid ethyl ester Natural products CCCCCC=CCC=CCCCCCCCC(=O)OCC FMMOOAYVCKXGMF-UHFFFAOYSA-N 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N n-hexanoic acid Natural products CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- 229960002446 octanoic acid Drugs 0.000 claims description 3
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 229940005605 valeric acid Drugs 0.000 claims description 3
- 239000012224 working solution Substances 0.000 claims description 3
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims description 2
- 239000003480 eluent Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- OWBTYPJTUOEWEK-ZXZARUISSA-N meso-butane-2,3-diol Chemical compound C[C@@H](O)[C@H](C)O OWBTYPJTUOEWEK-ZXZARUISSA-N 0.000 claims description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000003205 fragrance Substances 0.000 abstract description 2
- 235000020097 white wine Nutrition 0.000 abstract 4
- 239000004615 ingredient Substances 0.000 abstract 3
- 230000001476 alcoholic effect Effects 0.000 abstract 1
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 9
- 238000001514 detection method Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- PGMYKACGEOXYJE-UHFFFAOYSA-N pentyl acetate Chemical compound CCCCCOC(C)=O PGMYKACGEOXYJE-UHFFFAOYSA-N 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 150000005846 sugar alcohols Chemical class 0.000 description 6
- 230000035622 drinking Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- OXQGTIUCKGYOAA-UHFFFAOYSA-N 2-Ethylbutanoic acid Chemical compound CCC(CC)C(O)=O OXQGTIUCKGYOAA-UHFFFAOYSA-N 0.000 description 3
- 230000003204 osmotic effect Effects 0.000 description 3
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- 239000002253 acid Substances 0.000 description 2
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- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 description 2
- 238000013365 molecular weight analysis method Methods 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
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- 241000894006 Bacteria Species 0.000 description 1
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- 235000010469 Glycine max Nutrition 0.000 description 1
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Abstract
The invention discloses a kind of method for determining liquor flavor component synthesis molecular weight, belong to liquor flavor analysis technical field.51 kinds of volatility framework ingredient materials of main body are accounted in quantitative analysis white wine of the present invention, accounting of the material in totality is calculated with the molar concentration of every kind of material, then calculate the weighting molecular weight of volatile component;8 kinds of non-volatile alcoholic compounds of white wine generally existing with ion chromatography analysis, and accounting of the material in totality calculated with the molar concentration of every kind of material, then calculate the weighting molecular weight of nonvolatile element.The weighting molecular weight of the weighting molecular weight of volatility framework ingredient and non-volatilization component is added and obtained the synthesis molecule of white wine.Because this method to volatilize calculates obtained weighting molecular weight with the molar concentration of non-volatile framework ingredient, it can reflect that the bulk molecule amount of flavor and fragrance substance in white wine is horizontal comprehensively, foundation is provided for the molecular architecture and efficient and healthful of molecule Liquor Products.
Description
Technical Field
The invention relates to a method for measuring comprehensive molecular weight of flavor components of white spirit, belonging to the technical field of flavor analysis of white spirit.
Background
The diversity of Chinese liquor fermentation process forms the richness of liquor fragrance. Until now, 13 types of independent odor types recognized in the industry include faint scent type, strong odor type, Maotai odor type, rice odor type, mixed odor type, phoenix odor type, medicine (Dong) odor type, fermented soybean odor type, special odor type, sesame odor type, old and white dry odor type, strong odor type, pottery odor type and the like.
From a nutritional point of view, in general, relatively low molecular weight materials are more readily digested and absorbed. Therefore, an accurate comprehensive molecular weight detection method for Chinese liquor flavor substance systems is established, theoretical reference basis is provided for researching the comfort degree of the liquor before drinking, during drinking and after drinking, and the method has important significance.
At present, the molecular weight analysis methods commonly used in food are: an end group analysis method, a solution colligative method, an osmotic pressure method, a gas phase infiltration method, a viscosity method and the like, mainly inspect the average length distribution condition of short chains after pretreatment and hydrolysis of macromolecular polymers such as long-chain polysaccharide, polypeptide, fatty acid and the like, and provide a basis for optimizing the nutrition and the biological activity of the food. In food analysis, different methods are determined according to the difference of molecular weight and structure of polymers, the statistical significance and the application range of average molecular weight obtained by different methods are different, and the complexity of a solution and the accuracy of the method cause the method to have accuracy of only magnitude order. For example: the end group analysis method needs to define the functional group of a substance and can realize the quantification of the functional group, so that accurate molecular weight molecular analysis can be realized only by unifying the molecular attributes of short-chain substances as much as possible; the solution colligative method is applied to a nonvolatile and undissociated compound according to the physicochemical properties (heat capacity, boiling point, etc.) of the substance; the osmotic pressure method is used for measuring osmotic pressure phenomenon caused by chemical potential difference between solute and solution, and the molecular weight application range is 3 × 104Da-1×106Da range; the vapor permeation method is used for indirectly measuring the vapor pressure reduction of a solution to measure the average molecular weight of the solution, and the method has the advantages of less reagent dosage, high test speed and large error; the viscosity method is to calculate the molecular weight of the polymer according to the viscosity of the solution, and the method has simple equipment and simple operation, but the method requires a large degree of relation between the viscosity and the molecular weight of the solution, and only relative values are obtained by measurement.
The white spirit is a special flavor luxury product, the essence of the white spirit is a colloidal substance consisting of various flavor active substances such as alcohol aldehyde acid ester and the like, the average molecular weight of the spirit is between 100Da and 200Da, and in view of the complex spirit characteristics, the research on the comprehensive molecular weight cannot be realized by adopting a common physical and chemical method.
At present, no relevant research and report exists in the industry for an analysis method of comprehensive molecular weight in wine products. The industry only uses the concept of small molecules or micro molecules, but there is no definitive research conclusion on how to define, detect, and analyze and compare.
Disclosure of Invention
In order to solve the problems, the method disclosed by the invention is combined with a modern chromatographic analysis technology, adopts a molar concentration weighted molecular weight analysis method, accurately analyzes the comprehensive molecular weight of flavor substances in the white spirit, and has important significance for accurately inspecting the size of the total molecular weight of the white spirit and inspecting the structure and various functional characteristics of the white spirit body.
The invention aims to provide a method for measuring the comprehensive molecular weight of flavor components of white spirit. The main components of the white spirit are ethanol and water, and the total content of the ethanol and the water is about 97-99%; the alcohol, aldehyde, acid, ester and other various trace organic compounds dissolved in the wine only account for 1-3% of the total amount; the trace amount of aroma and flavor substances with the content of only 1-3% is the key for determining the aroma, taste and style of the white spirit; among these minor components, there are two categories: volatile components and non-volatile components. Therefore, the method measures the comprehensive molecular weight of the white spirit from two aspects of volatilization and non-volatilization, and comprehensively calculates the weighted molecular weight of the flavor substances of the white spirit by taking 51 kinds of ubiquitous volatile skeleton flavors of the white spirit (the 51 kinds of substances comprise the substances of skeleton components of the white spirit confirmed in the industry, namely, the content is more than 20-30 mg/L) and 8 kinds of ubiquitous sugar alcohol nonvolatile components in the white spirit (the 8 kinds of substances are 8 kinds of nonvolatile substances with the highest ion chromatographic analysis content) as main bodies. The yield of the polyhydric alcohol is closely related to strains, the number of bacteria, raw materials, the fermentation speed, the fermented grain components and the like, and the polyhydric alcohol in the white spirit mainly comprises eight types of glycerol, erythritol, xylitol, arabitol, sorbitol, galactitol, mannitol and maltitol according to the characteristics of samples.
In the invention, the molar concentration of each key substance in the liquor body is used, because the molar concentration represents the molecular number of the substance in the solution, the arrangement and the proportion of the substance in the liquor body can be reflected, and the total flavor substance molecular weight of the white liquor can be determined more accurately by adopting a weighting (%) method:
the weighted molecular weight ═ sigma skeleton component molar concentration ratio (%) × skeleton component molecular weight
The method for measuring the comprehensive molecular weight of the flavor components of the white spirit comprises the following steps:
(1) measuring the mass concentration (mg/L) of volatile skeleton components in the white spirit;
(2) calculating the weighted molecular weight of volatile skeleton components in the white spirit; wherein,
the weighted molecular weight of the volatile skeleton component in the white spirit is ═ Sigma molar concentration ratio (%) of the volatile skeleton component and the molecular weight of the skeleton component
A molar concentration ratio (%) of the volatile skeleton component (M mol/total mol) of the volatile skeleton component
Molar concentration M (mol/L) of volatile skeleton component (mass concentration of the substance)/molecular weight of the substance
Total molar concentration (mol/L) of volatile skeleton components (sum of molar concentrations of 51 or more volatile skeleton components)
(3) Measuring the mass concentration (mg/L) of non-volatile skeleton components in the white spirit;
(4) calculating the weighted molecular weight of the non-volatile framework components in the white spirit; wherein,
weight ratio (%) of mole concentration of non-volatile skeleton component ═ Σ of mole concentration of non-volatile skeleton component in white spirit and molecular weight of skeleton component
Molar concentration ratio (%) of non-volatile skeleton component to total molar concentration of non-volatile skeleton component
Molar concentration of non-volatile skeleton component M (mol/L) ═ mass concentration of the substance/molecular weight of the substance
The total molar concentration M (mol/L) of the non-volatile skeleton components is the sum of the molar concentrations of more than 8 kinds of sugar alcohol non-volatile skeleton components
(5) Calculating the comprehensive molecular weight of the flavor components of the white spirit:
the comprehensive molecular weight of the flavor components of the white spirit is the weighted molecular weight of volatile skeleton components in the white spirit and the weighted molecular weight of non-volatile skeleton components in the white spirit.
In one embodiment, the volatile matrix component comprises acetaldehyde, n-propionaldehyde, ethyl formate, ethyl acetate, acetal, methanol, isovaleraldehyde, 2-pentanone, ethyl butyrate, sec-butanol, n-propanol, 1-diethoxy-2-methylbutane, 1-diethoxy-3-methylbutane, isobutanol, isoamyl acetate, ethyl valerate, 2-pentanol, n-butanol, 2-methyl-1-butanol, isoamyl alcohol, ethyl hexanoate, n-pentanol, 3-hydroxy-2-butanone, ethyl heptanoate, ethyl lactate, n-hexanoate, butyl hexanoate, ethyl octanoate, isoamyl hexanoate, acetic acid, furfural, benzaldehyde, propionic acid, 2, 3-butanediol (levo), isobutyric acid, 2, 3-butanediol (meso-butanol), propylene glycol, ethyl decanoate, butyric acid, furfuryl alcohol, isovaleric acid, valeric acid, ethyl phenylacetate, hexanoic acid, β -phenylethyl alcohol, heptanoic acid, ethyl tetradecanoate, caprylic acid, ethyl palmitate, ethyl oleate, ethyl linoleate.
The invention also provides the determination of the volatile framework components, which adopts gas chromatography to carry out quantitative analysis.
In one embodiment, the gas chromatography conditions are: adopting a capillary column, wherein the temperature of a sample inlet is 210-250 ℃; the initial column temperature is 30-40 ℃, the temperature is raised to 55-65 ℃ at 1-3 ℃/min, the temperature is kept for 2-6min, the temperature is raised to 210 ℃ at 4-8 ℃/min, and the temperature is kept for 15-25 min; the carrier gas is inert gas; the flow rate is 0.5-2 mL/min; the sample introduction mode is split-flow sample introduction.
In one embodiment, the split ratio of the split feed is 20:1 to 40: 1.
The instrument comprises the following steps: agilent 7890B gas chromatograph (FID detector);
chromatographic conditions are as follows: the chromatographic column is Agilent CP-Wax 57CB capillary column [50m × 0.25mm (inner diameter) × 0.2 μm ]; the temperature of a sample inlet is 230 ℃; the initial column temperature is 35 ℃, the temperature is raised to 60 ℃ at the speed of 2 ℃/min, the temperature is kept for 4min, the temperature is raised to 195 ℃ at the speed of 6 ℃/min, and the temperature is kept for 20 min; the carrier gas is nitrogen, and the purity is not less than 99.999 percent; the flow rate is 1 mL/min; the sample injection mode is divided sample injection, and the dividing ratio is 30: 1; the injection volume was 1. mu.L.
In one embodiment, the specific conditions of the gas chromatograph are:
the instrument comprises the following steps: agilent 7890B gas chromatograph (FID detector);
chromatographic conditions are as follows: the chromatographic column is Agilent CP-Wax 57CB capillary column [50m × 0.25mm (inner diameter) × 0.2 μm ]; the temperature of a sample inlet is 230 ℃; the initial column temperature is 35 ℃, the temperature is raised to 60 ℃ at the speed of 2 ℃/min, the temperature is kept for 4min, the temperature is raised to 195 ℃ at the speed of 6 ℃/min, and the temperature is kept for 20 min; the carrier gas is nitrogen, and the purity is not less than 99.999 percent; the flow rate is 1 mL/min; the sample injection mode is divided sample injection, and the dividing ratio is 30: 1; the injection volume was 1. mu.L.
In one embodiment, the quantitative analysis by gas chromatography is performed by preparing standard substances of the same framework component with different concentrations, adding an internal standard with a certain concentration to prepare a standard working solution with gradient concentration, and performing gas chromatography analysis to obtain a standard curve of each framework component; and substituting the meteorological chromatographic analysis result of the sample to be detected into the standard curve to obtain the content of the sample to be detected.
In one embodiment, the non-volatile framework composition comprises: glycerol, erythritol, xylitol, arabitol, sorbitol, galactitol, mannitol, maltitol.
The invention also provides the determination of the non-volatile framework components, which adopts ion chromatography to carry out quantitative analysis.
In one embodiment, the ion chromatography conditions are: the temperature of the chromatographic column is 25-35 ℃; the leacheate is NaOH solution, and the flow rate is 0.2-0.6 mL/min.
In one embodiment, the ion chromatography conditions are: the ion chromatograph is ICS-5000+, and is provided with an ampere detector, an Au working electrode and an Ag reference electrode; the chromatographic column is CarboPac MA1, and the column temperature is 30 ℃; the eluent is 480mM NaOH, and the flow rate is 0.4 mL/min; the amount of sample was 25. mu.L. The method is obtained by experimental optimization and is suitable for analyzing the polyhydric alcohol in the white spirit sample.
The invention has the beneficial effects that:
1. the method of the invention determines the comprehensive molecular weight of the white spirit by carrying out quantitative analysis on the volatile skeleton components and the non-volatile skeleton components in the white spirit, and then respectively calculating the weighted molecular weight of each substance according to the molar concentration ratio of each substance. The method calculates the weighted molecular weight according to the molar concentration of the skeleton components in the white spirit, and reflects the molecular weight of the product on the whole.
2. The invention is a comprehensive algorithm for combining the weighted molecular weight of the volatile skeleton component and the non-volatile skeleton component in the white spirit for the first time, and can more comprehensively reflect the comprehensive molecular weight of the white spirit product.
3. The invention provides a method for calculating the comprehensive molecular weight of the white spirit for the first time, and provides reference for knowing the overall molecular weight state and distribution of flavor substances in the white spirit.
Drawings
FIG. 1: a standard curve for ethyl hexanoate detection;
FIG. 2: an example of a whole chromatogram;
FIG. 3: a standard curve for glycerol detection;
FIG. 4: spectra of standard samples of 8 non-volatile components.
Detailed description of the preferred embodiments
The present invention will be described in detail below.
Example 1
The comprehensive molecular weight of the flavor components of the white spirit is measured according to the following method:
dividing a sample into two parts, respectively analyzing volatile skeleton components and non-volatile skeleton components, respectively calculating the weighted molecular weight of the volatile skeleton components in the white spirit and the weighted molecular weight of the non-volatile skeleton components in the white spirit, and finally obtaining the comprehensive molecular weight of the flavor components of the white spirit.
The method comprises the following specific steps:
(1) determination of mass concentration of volatile skeleton components in white spirit (mg/L):
the detection method comprises the following steps:
a, instruments: agilent 7890B gas chromatograph (FID detector)
b, reagent: tert-amyl alcohol, n-amyl acetate and 2-ethyl butyric acid chromatographic standard substance (content is not less than 99.5%, Tianjin City shin-repairing fine chemical research institute)
c, chromatographic conditions: a chromatographic column: agilent CP-Wax 57CB capillary column [50m × 0.25mm (inner diameter) × 0.2 μm ], injection port temperature 230 ℃; carrier gas: the purity of nitrogen is not less than 99.999%; flow rate: 1 mL/min; and (3) sample introduction mode: split-flow sample introduction, split-flow ratio: 30: 1; sample introduction volume: 1 μ L.
d, establishing a standard curve: respectively sucking 10mL of skeleton component mixed standard substance with gradient concentration, and adding 10 μ L of mixed internal standard (tert-amyl alcohol, n-amyl acetate and 2-ethyl butyric acid standard solution) with certain concentration to prepare standard working solution with gradient concentration. Collecting signals under the chromatographic conditions, respectively taking tert-amyl alcohol, n-amyl acetate and 2-ethyl butyric acid as internal standards, and drawing a standard curve of each component by using an off-line workstation.
Taking ethyl caproate as an example: the standard curve is that y is 1.01789x (y is a peak area ratio, x is a content ratio), the linear correlation coefficient is 0.9996 (figure 1), and the recovery rate of the two points of the measured concentration of 352.23mg/L and 2817.8mg/L is between 80% and 120%.
Acetaldehyde, n-propionaldehyde, ethyl formate, ethyl acetate, acetal, methanol, isovaleraldehyde, 2-pentanone, ethyl butyrate, sec-butanol, n-propanol, 1-diethoxy-2-methylbutane, 1-diethoxy-3-methylbutane, isobutanol, isoamyl acetate, ethyl valerate, 2-pentanol, n-butanol, 2-methyl-1-butanol, isoamyl alcohol, ethyl hexanoate, n-pentanol, 3-hydroxy-2-butanone, ethyl heptanoate, ethyl lactate, n-hexanoate, butyl hexanoate, ethyl octanoate, isoamyl hexanoate, acetic acid, furfural, benzaldehyde, propionic acid, 2, 3-butanediol (levo), isobutyric acid, 2, 3-butanediol (meso), propylene glycol, ethyl decanoate, butyric acid, furfuryl alcohol, isovaleric acid, valeric acid, ethyl phenylacetate, hexanoic acid, β -phenylethyl alcohol, heptanoic acid, ethyl tetradecanoate, octanoic acid, ethyl palmitate, ethyl oleate, ethyl linoleate.
An example of a whole chromatogram is shown in FIG. 2. Wherein, the linear correlation coefficients of the detection of 51 substances by adopting the gas chromatography for direct sample injection and the FID detector are all above 0.99, and the recovery rate is all between 80 and 120 percent.
(2) Calculation of weighted molecular weight of volatile skeleton components in white spirit
The weighted molecular weight of the volatile skeleton component of the white spirit ═ sigma skeleton component molar concentration ratio (%) × skeleton component molecular weight volatile skeleton component molar concentration ratio (%) ═ mol concentration of the component M/total mol concentration of the volatile skeleton component
Total molar concentration (mol/L) of 51 volatile components molar concentration and the molar concentration M (mol/L) of the volatile skeleton component is the mass concentration/molecular weight of the substance
(3) Determination of mass concentration of non-volatile skeleton components in white spirit (mg/L):
the ion chromatography is adopted to carry out quantitative analysis on 8 non-volatile framework components represented by sugar alcohols in the white spirit: glycerol, erythritol, xylitol, arabitol, sorbitol, galactitol, mannitol, maltitol.
The detection method comprises the following steps:
ion chromatography: ICS-5000+, equipped with amperometric detector, Au working electrode, Ag reference electrode;
a chromatographic column: CarboPac MA1, column temperature: 30 ℃;
leacheate: 480mm naoh, flow rate: 0.4 ml/min;
sample introduction amount: 25 μ L.
The standard curve is shown in FIG. 3, using glycerol as an example.
The spectrum of the standard sample of the composition in 8 under the detection conditions of this example is shown in FIG. 4, and the coefficients of the standard curve are shown in Table 1. Further, the inventors performed a recovery rate test, and the results are shown in table 2. As can be seen from the table 1-2, the linearity of each component coefficient is above 0.9997, and the recovery rate of the added standard is between 85% and 102%, which shows that the ion chromatography detection effect is good.
Table 1 standard curve coefficients for each component:
serial number | Component name | Linearity | Serial number | Name (R) | Linearity |
1 | Glycerol | 0.9999 | 5 | Sorbitol | 0.9999 |
2 | Erythritol and its preparation method | 0.9998 | 6 | Galactitol | 0.9998 |
3 | Xylitol, its preparation method and use | 0.9999 | 7 | Mannitol | 0.9999 |
4 | Arabinol | 0.9999 | 8 | Maltitol | 0.9997 |
TABLE 2 recovery of the components
Serial number | Component name | Standard concentration (mg/L) | Test results (mg/L) | Recovery (%) |
1 | Glycerol | 0.52 | 0.53 | 101.92 |
2 | Erythritol and its preparation method | 0.46 | 0.39 | 84.78 |
3 | Xylitol, its preparation method and use | 0.36 | 0.32 | 88.89 |
4 | Arabinol | 0.50 | 0.49 | 98.00 |
5 | Sorbitol | 0.42 | 0.39 | 92.86 |
6 | Galactitol | 0.40 | 0.33 | 82.50 |
7 | Mannitol | 0.56 | 0.48 | 85.71 |
8 | Maltitol | 0.56 | 0.52 | 92.86 |
Remarking: the background content is deducted from the detection result.
(4) Calculation of weighted molecular weight of non-volatile skeleton components in white spirit
The weighted molecular weight of non-volatile skeleton component in white spirit is ═ sigma skeleton component mol concentration ratio (%) × skeleton component molecular weight
Molar concentration ratio (%) of non-volatile skeleton component (M) to total molar concentration of the non-volatile skeleton component
Molar concentration M (mol/L) of non-volatile skeleton component (mass concentration/molecular weight of the substance)
Total molar concentration (mol/L) of the sum of the molar concentrations of 8 non-volatile components
(5) Calculating the comprehensive molecular weight of the white spirit:
the comprehensive molecular weight of the white spirit is the weighted molecular weight of the volatile skeleton components in the white spirit and the weighted molecular weight of the non-volatile skeleton components in the white spirit
The comprehensive molecular weight of the flavor components of the white spirit measured by the method comprehensively and effectively reflects the overall molecular weight level of the flavor-developing substances in the white spirit, and the white spirit with small comprehensive molecular weight is easier to digest and absorb than the white spirit with relatively larger comprehensive molecular weight, can be used for evaluating the metabolic easiness of the spirit body, provides a theoretical reference basis for researching the comfort degree of the white spirit before, during and after drinking, and has important significance.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for measuring comprehensive molecular weight of flavor components of white spirit is characterized by comprising the following steps:
(1) measuring the mass concentration of volatile skeleton components in the white spirit;
(2) calculating the weighted molecular weight of volatile skeleton components in the white spirit; wherein,
the weighted molecular weight of the volatile skeleton component in the white spirit is ═ Sigma molar concentration ratio (%) of the volatile skeleton component and the molecular weight of the skeleton component
A molar concentration ratio (%) of the volatile skeleton component (M mol/total mol) of the volatile skeleton component
Molar concentration M (mol/L) of volatile skeleton component (mass concentration of the substance)/molecular weight of the substance
(3) Measuring the mass concentration of non-volatile skeleton components in the white spirit;
(4) calculating the weighted molecular weight of the non-volatile framework components in the white spirit; wherein,
weight ratio (%) of mole concentration of non-volatile skeleton component ═ Σ of mole concentration of non-volatile skeleton component in white spirit and molecular weight of skeleton component
Molar concentration ratio (%) of non-volatile skeleton component to total molar concentration of non-volatile skeleton component
Molar concentration of non-volatile skeleton component M (mol/L) ═ mass concentration of the substance/molecular weight of the substance
(5) Calculating the comprehensive molecular weight of the flavor components of the white spirit:
the comprehensive molecular weight of the flavor components of the white spirit is the weighted molecular weight of volatile skeleton components in the white spirit and the weighted molecular weight of non-volatile skeleton components in the white spirit.
2. The method of claim 1, wherein the volatile matrix component comprises acetaldehyde, n-propionaldehyde, ethyl formate, ethyl acetate, acetal, methanol, isovaleraldehyde, 2-pentanone, ethyl butyrate, sec-butanol, n-propanol, 1-diethoxy-2-methylbutane, 1-diethoxy-3-methylbutane, isobutanol, isoamyl acetate, ethyl valerate, 2-pentanol, n-butanol, 2-methyl-1-butanol, isoamyl alcohol, ethyl hexanoate, n-pentanol, 3-hydroxy-2-butanone, ethyl heptanoate, ethyl lactate, n-hexanol, butyl hexanoate, ethyl octanoate, isoamyl hexanoate, acetic acid, furfural, benzaldehyde, propionic acid, 2, 3-butanediol (levo), isobutyric acid, 2, 3-butanediol (meso), propylene glycol, ethyl decanoate, butyric acid, furfuryl alcohol, isovaleric acid, valeric acid, ethyl phenylacetate, hexanoic acid, β -phenylethyl alcohol, heptanoic acid, ethyl tetradecanoate, caprylic acid, ethyl palmitate, ethyl oleate, linoleic acid, ethyl linoleate.
3. The method of claim 1, wherein the non-volatile framework components comprise: glycerol, erythritol, xylitol, arabitol, sorbitol, galactitol, mannitol, maltitol.
4. The method of claim 1, wherein the volatile matrix composition is determined quantitatively using gas chromatography.
5. The method of claim 1, wherein the non-volatile framework components are determined quantitatively by ion chromatography.
6. The method according to claim 4, wherein the quantitative analysis by gas chromatography comprises preparing standard substances of the same skeleton component with different concentrations, adding an internal standard with a certain concentration to prepare a standard working solution with a gradient concentration, and performing gas chromatography to obtain a standard curve of each skeleton component; and substituting the meteorological chromatographic analysis result of the sample to be detected into the standard curve to obtain the content of the sample to be detected.
7. The method according to claim 4, characterized in that the conditions of the gas chromatography are: adopting a capillary column, wherein the temperature of a sample inlet is 210-250 ℃; the initial column temperature is 30-40 ℃, the temperature is raised to 55-65 ℃ at 1-3 ℃/min, the temperature is kept for 2-6min, the temperature is raised to 210 ℃ at 4-8 ℃/min, and the temperature is kept for 15-25 min; the carrier gas is inert gas; the flow rate is 0.5-2 mL/min; the sample introduction mode is split-flow sample introduction.
8. The method according to claim 4, characterized in that the specific conditions of the gas chromatograph are:
the instrument comprises the following steps: agilent 7890B gas chromatograph (FID detector);
chromatographic conditions are as follows: the chromatographic column is Agilent CP-Wax 57CB capillary column [50m × 0.25mm (inner diameter) × 0.2 μm ]; the temperature of a sample inlet is 230 ℃; the carrier gas is nitrogen, and the purity is not less than 99.999 percent; the flow rate is 1 mL/min; the sample injection mode is divided sample injection, and the dividing ratio is 30: 1; the injection volume was 1. mu.L.
9. The method of claim 5, wherein the conditions of the ion chromatography are: the conditions of the ion chromatography are: the temperature of the chromatographic column is 25-35 ℃; the leacheate is NaOH solution, and the flow rate is 0.2-0.6 mL/min.
10. The method of claim 5, wherein the conditions of the ion chromatography are: the ion chromatograph is ICS-5000+, and is provided with an ampere detector, an Au working electrode and an Ag reference electrode; the chromatographic column is CarboPac MA1, and the column temperature is 30 ℃; the eluent is 480mM NaOH, and the flow rate is 0.4 mL/min; the amount of sample was 25. mu.L.
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