CN109632987A - 一种快速检测芳樟醇含量的方法 - Google Patents
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- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000001514 detection method Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 title claims abstract description 26
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 title claims abstract description 26
- 229930007744 linalool Natural products 0.000 title claims abstract description 26
- 241000723346 Cinnamomum camphora Species 0.000 claims abstract description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000341 volatile oil Substances 0.000 claims abstract description 19
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims abstract description 12
- 239000012085 test solution Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001256 steam distillation Methods 0.000 claims abstract description 4
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 abstract description 8
- 238000004817 gas chromatography Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000009395 breeding Methods 0.000 description 5
- 230000001488 breeding effect Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- CDOSHBSSFJOMGT-SNVBAGLBSA-N (S)-linalool Chemical compound CC(C)=CCC[C@](C)(O)C=C CDOSHBSSFJOMGT-SNVBAGLBSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000002360 explosive Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000010200 validation analysis Methods 0.000 description 3
- FUDNBFMOXDUIIE-UHFFFAOYSA-N 3,7-dimethylocta-1,6-diene Chemical group C=CC(C)CCC=C(C)C FUDNBFMOXDUIIE-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000010829 isocratic elution Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- PXRCIOIWVGAZEP-UHFFFAOYSA-N Camphene hydrate Chemical compound C1CC2C(O)(C)C(C)(C)C1C2 PXRCIOIWVGAZEP-UHFFFAOYSA-N 0.000 description 1
- 241000723347 Cinnamomum Species 0.000 description 1
- 241000218195 Lauraceae Species 0.000 description 1
- 239000010692 aromatic oil Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000000105 evaporative light scattering detection Methods 0.000 description 1
- 238000003859 hyphenated technique Methods 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 terpene Enol Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
本发明公开一种快速检测芳樟醇含量的方法,该方法采用液相色谱法检测芳樟醇含量,其步骤如下:用水蒸汽蒸馏法提取芳香樟精油,精确称取香樟精油41.5mg,置10mL容量瓶中,采用甲醇定溶,即得供试品溶液,供试品溶液的精油含量控制在≦5mg/mL;采用高效液相色谱仪检测,色谱柱为C18色谱柱、150×4.6nm、5μm,柱温30℃,流速1.0 ml,流动相甲醇:水为70:30,检测波长:210 nm,进样量10μl,检测时间:12 min,即可精确检测出芳香醇的含量;该方法分离度好,稳定性强、重现性高、精确度好,比现有采用GC和GC‑MS的方法设备及技术操作更为简单、安全、对操作人员技术要求低,用时短主。
Description
技术领域
本发明专利涉及一种快速检测芳樟醇含量的方法。
背景技术
香樟,Cinamomum camphoravar. Linaloolifera又名樟树、芳樟、乌樟等,是樟科樟属常绿高大乔木。香樟中含有大量精油,是医药、化工、香料工业的重要原料。在香樟的精油中,存在天然的芳樟醇。芳樟醇(Linalool)又名沉香醇、芫荽醇、伽罗木醇、里那醇等,学名是3,7-二甲基-1,6辛二烯-3-醇,分子式为C10H18O,分子量为154.24。芳樟醇属于链状萜烯醇类,有α-和β-两种异构体。当今人们崇尚大自然,芳樟醇的香气大行其道,因此,芳樟醇广泛应用于香料、香精、香水、古龙水、香皂中,在单体芳香油中占有重要地位,素有“香料大王”美称。培育具有高含量、高纯度芳樟醇的香樟品种已成为当下香樟品系选育的研究热点。而在具有高含量、高纯度芳樟醇的香樟品种选育研究中,香樟中芳樟醇的含量测定方法是品种选育的关键环节。
目前,香樟中芳樟醇含量的检测方法是利用精油的挥发性,采用气相色谱法(GC)或气相-质谱联用技术(GC-MS)等进行检测,主要是由于精油属于挥发性物质,传统理论认为高效液相色谱法在检测精油过程中含量会有损失,造成检测不准确,检测误差大于1%,且方法学验证中稳定性无法达到检测要求,因此,限制了该方法在精油检测中的应用。然而,GC及GC-MS色谱法在当下的应用过程中面临诸多问题。GC及GC-MS色谱仪价格昂贵,对实验室的要求高;生产单位或基层事新品种选育研究的机构的此类仪器的配置率低,GC-MS联用仪更是无从谈起,这极大限制了基层技术人员在该领域的研发进程或质量跟踪管理;且GC及GC-MS操作较为繁琐,需耗费大量的时间在仪器的平衡过程,分离过程往往采取程序升温方式、计算中又需结合内标法,且在检测过程中需用氮气及氢气等易燃易爆气体,危险系数大,分析成本高,对基层技术人员的技术要求高,基层科技工作者很难掌握该检测方法。而基层生产单位或科研机构的高效液相色谱仪配备率高,使用技术也掌握的比较好,
基于此,生产中急需要有一种快速检测芳樟醇含量的方法,该方法所使用的高效液相色谱仪、检测方法操作简单,时间短、对操作人员技术要求较现有技术低。
发明内容
本发明旨在提供一种利用高效液相色谱仪快速检测芳樟醇含量的方法,且色谱洗脱方法简单,不需要氮气及氢气等易燃易爆气体,只需等度洗脱无需复杂梯度和程序升温,用时短,工作效率高,显著优于现有技术。
本发明提供的技术方案为:一种快速检测芳樟醇含量的方法,其液相色谱法检测芳樟醇含量,包括以下步骤。
采用水蒸汽蒸馏法提取芳香樟精油,精确称取香樟精油41.5mg,置10mL容量瓶中,采用甲醇定溶,即得供试品溶液,供试品溶液精油含量控制在≦5mg/mL;
将供试品溶液采用液相色谱法分析;
仪器:高效液相色谱仪;
色谱柱:C18 色谱柱,150×4.6nm,5μm;
柱温:30℃;
流速:1.0 ml;
流动相:甲醇:水为70:30
检测波长:210 nm;
进样量:10 μl;
芳樟醇的保留时间:9.2 min
检测时间:12 min,即可精确检测出芳香醇含量。
方法学验证结果:精密度的RSD为0.39%,重复性RSD为1.93%,样品在12小时内稳定性RSD为0.98%,加样回收率实验的回收率在95.3%-98.2%之间,结果表明,该检测方法精确度高、重现性及稳定性好。
本发明的一种快速检测芳樟醇含量的方法与现有GC和GC-MS检测芳香樟、芳香樟精油中芳樟醇的技术相比其显著优点在于:
1、液相色谱法检测中所使用到的试剂为甲醇和水,比气相色谱使用的易燃易爆气体更安全,对技术人员的要求更低;
2、本专利对供试品溶液配制浓度进行深入的探索。当供试品溶液精油含量控制在5mg/mL 浓度以下时,芳香樟精油挥发性造成的损失在±1%的误差范围内,且方法学验证中,样品在12小时内稳定,其RSD值均小于1%,克服了人们认为高效液相色谱法在检测挥发精油过程中含量会有损失,造成检测不准确的误差。
3、已报道的GC和GC-MS检测时间在35-60min,本方法检测时间仅需12min,显著的缩短时间,提高效率,更加符合基层品种选育大批量检测的要求。
因此本发明所提供的一种利用高效液相色谱仪快速检测芳樟醇含量的方法,色谱洗脱方法简单,不需要氮气及氢气等易燃易爆气体,只需等度洗脱无需复杂梯度和程序升温,用时短,工作效率高,显著优于现有技术。
以下将结合实施例对发明作进一步叙述:
实施例1
采用水蒸汽蒸馏法提取芳香樟精油,精确称取香樟精油41.5mg,在10mL容量瓶中用甲醇定溶,即得供试品溶液;将供试品溶液采用液相色谱法分析; 色谱柱:C18 色谱柱,150×4.6nm,5μm;柱温:30℃;流速:1.0 ml;流动相:甲醇:水为70:30检测波长:210 nm;进样量:10 μl;芳樟醇的保留时间:9.2 min检测时间:12 min即可精确检测出芳香醇含量。
经检验该检测实施例精密度的RSD为0.39%,重复性RSD为1.93%,样品在12小时内稳定性RSD为0.98%,加样回收率实验的回收率在95.3%-98.2%之间,结果表明,该检测方法精确度高、重现性及稳定性好。
Claims (1)
1.一种快速检测芳樟醇含量的方法,其特征是采用液相色谱法检测,包括以下步骤:(1)
采用水蒸汽蒸馏法提取芳香樟精油,精确称取香樟精油41.5mg,置10mL容量瓶中,采用甲醇定溶,即得供试品溶液,供试品溶液的精油含量控制在≦5mg/mL;采用高效液相色谱仪检测,色谱柱为C18 色谱柱、150×4.6nm、5μm,柱温30℃,流速1.0 ml,流动相甲醇:水为70:30,检测波长:210 nm,进样量10 μl,检测时间:12 min,即可精确检测出芳香醇的含量。
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CN115452981A (zh) * | 2022-09-05 | 2022-12-09 | 云南中烟工业有限责任公司 | 一种基于gc-ms的野坝子不同药用部位的线性判别方法 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8372646B1 (en) * | 2009-12-21 | 2013-02-12 | Medtronic Minimed, Inc. | Terpene media compositions for eluting compounds from matrices and methods for making and using them |
CN108998383A (zh) * | 2017-06-06 | 2018-12-14 | 华东理工大学 | 一种产芳樟醇的解脂耶氏酵母基因工程菌及其应用 |
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Publication number | Priority date | Publication date | Assignee | Title |
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US8372646B1 (en) * | 2009-12-21 | 2013-02-12 | Medtronic Minimed, Inc. | Terpene media compositions for eluting compounds from matrices and methods for making and using them |
CN108998383A (zh) * | 2017-06-06 | 2018-12-14 | 华东理工大学 | 一种产芳樟醇的解脂耶氏酵母基因工程菌及其应用 |
Non-Patent Citations (3)
Title |
---|
EN-QIN XIA等: "A New High-Performance Liquid Chromatographic Method for the Determination and Distribution of Linalool in Michelia alba" * |
MANOJ K DALAI等: "Anti-cholinesterase potential of Cinnamomum tamala (Buch.-Ham.) T.Nees & Eberm. leaves" * |
欧可可等: "不同时期花生茎叶中芳樟醇含量的测定" * |
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CN115452981A (zh) * | 2022-09-05 | 2022-12-09 | 云南中烟工业有限责任公司 | 一种基于gc-ms的野坝子不同药用部位的线性判别方法 |
CN115452981B (zh) * | 2022-09-05 | 2024-02-23 | 云南中烟工业有限责任公司 | 一种基于gc-ms的野坝子不同药用部位的线性判别方法 |
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