JPS6223256B2 - - Google Patents
Info
- Publication number
- JPS6223256B2 JPS6223256B2 JP53130900A JP13090078A JPS6223256B2 JP S6223256 B2 JPS6223256 B2 JP S6223256B2 JP 53130900 A JP53130900 A JP 53130900A JP 13090078 A JP13090078 A JP 13090078A JP S6223256 B2 JPS6223256 B2 JP S6223256B2
- Authority
- JP
- Japan
- Prior art keywords
- carrier
- diatomaceous earth
- packing material
- stationary phase
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000005909 Kieselgur Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 12
- 230000005526 G1 to G0 transition Effects 0.000 claims description 11
- 229920002472 Starch Polymers 0.000 claims description 6
- 235000019698 starch Nutrition 0.000 claims description 6
- 239000008107 starch Substances 0.000 claims description 6
- 239000000523 sample Substances 0.000 description 12
- ZCTQGTTXIYCGGC-UHFFFAOYSA-N Benzyl salicylate Chemical compound OC1=CC=CC=C1C(=O)OCC1=CC=CC=C1 ZCTQGTTXIYCGGC-UHFFFAOYSA-N 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 238000004817 gas chromatography Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000003205 fragrance Substances 0.000 description 7
- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- QMVPMAAFGQKVCJ-UHFFFAOYSA-N citronellol Chemical compound OCCC(C)CCC=C(C)C QMVPMAAFGQKVCJ-UHFFFAOYSA-N 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- SESFRYSPDFLNCH-UHFFFAOYSA-N benzyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC1=CC=CC=C1 SESFRYSPDFLNCH-UHFFFAOYSA-N 0.000 description 4
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- QMVPMAAFGQKVCJ-SNVBAGLBSA-N (R)-(+)-citronellol Natural products OCC[C@H](C)CCC=C(C)C QMVPMAAFGQKVCJ-SNVBAGLBSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000005792 Geraniol Substances 0.000 description 3
- GLZPCOQZEFWAFX-YFHOEESVSA-N Geraniol Natural products CC(C)=CCC\C(C)=C/CO GLZPCOQZEFWAFX-YFHOEESVSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- JGQFVRIQXUFPAH-UHFFFAOYSA-N beta-citronellol Natural products OCCC(C)CCCC(C)=C JGQFVRIQXUFPAH-UHFFFAOYSA-N 0.000 description 3
- 235000000484 citronellol Nutrition 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 229940113087 geraniol Drugs 0.000 description 3
- -1 phthalate ester Chemical class 0.000 description 3
- 229920001592 potato starch Polymers 0.000 description 3
- 125000005372 silanol group Chemical group 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- FACFHHMQICTXFZ-UHFFFAOYSA-N 2-(2-phenylimidazo[1,2-a]pyridin-3-yl)ethanamine Chemical compound N1=C2C=CC=CN2C(CCN)=C1C1=CC=CC=C1 FACFHHMQICTXFZ-UHFFFAOYSA-N 0.000 description 2
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 description 2
- 241000402754 Erythranthe moschata Species 0.000 description 2
- 239000005770 Eugenol Substances 0.000 description 2
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 description 2
- KGEKLUUHTZCSIP-HOSYDEDBSA-N [(1s,4s,6r)-1,7,7-trimethyl-6-bicyclo[2.2.1]heptanyl] acetate Chemical compound C1C[C@]2(C)[C@H](OC(=O)C)C[C@H]1C2(C)C KGEKLUUHTZCSIP-HOSYDEDBSA-N 0.000 description 2
- 229960002903 benzyl benzoate Drugs 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- JOZKFWLRHCDGJA-UHFFFAOYSA-N citronellol acetate Chemical compound CC(=O)OCCC(C)CCC=C(C)C JOZKFWLRHCDGJA-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229960002217 eugenol Drugs 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 2
- UWKAYLJWKGQEPM-LBPRGKRZSA-N linalyl acetate Chemical compound CC(C)=CCC[C@](C)(C=C)OC(C)=O UWKAYLJWKGQEPM-LBPRGKRZSA-N 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229940067137 musk ketone Drugs 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N squalane Chemical compound CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 2
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 description 1
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 description 1
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 1
- VPKMGDRERYMTJX-CMDGGOBGSA-N 1-(2,6,6-Trimethyl-2-cyclohexen-1-yl)-1-penten-3-one Chemical compound CCC(=O)\C=C\C1C(C)=CCCC1(C)C VPKMGDRERYMTJX-CMDGGOBGSA-N 0.000 description 1
- CHLICZRVGGXEOD-UHFFFAOYSA-N 1-Methoxy-4-methylbenzene Chemical compound COC1=CC=C(C)C=C1 CHLICZRVGGXEOD-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- JOZKFWLRHCDGJA-LLVKDONJSA-N Citronellyl acetate Natural products CC(=O)OCC[C@H](C)CCC=C(C)C JOZKFWLRHCDGJA-LLVKDONJSA-N 0.000 description 1
- KBEBGUQPQBELIU-CMDGGOBGSA-N Ethyl cinnamate Chemical compound CCOC(=O)\C=C\C1=CC=CC=C1 KBEBGUQPQBELIU-CMDGGOBGSA-N 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- KVWWIYGFBYDJQC-GHMZBOCLSA-N Methyl dihydrojasmonate Chemical compound CCCCC[C@@H]1[C@@H](CC(=O)OC)CCC1=O KVWWIYGFBYDJQC-GHMZBOCLSA-N 0.000 description 1
- 229920000294 Resistant starch Polymers 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 description 1
- 229940088601 alpha-terpineol Drugs 0.000 description 1
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N benzo-alpha-pyrone Natural products C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 1
- 229940115397 bornyl acetate Drugs 0.000 description 1
- KBEBGUQPQBELIU-UHFFFAOYSA-N cinnamic acid ethyl ester Natural products CCOC(=O)C=CC1=CC=CC=C1 KBEBGUQPQBELIU-UHFFFAOYSA-N 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- SDQFDHOLCGWZPU-UHFFFAOYSA-N lilial Chemical compound O=CC(C)CC1=CC=C(C(C)(C)C)C=C1 SDQFDHOLCGWZPU-UHFFFAOYSA-N 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- UWKAYLJWKGQEPM-UHFFFAOYSA-N linalool acetate Natural products CC(C)=CCCC(C)(C=C)OC(C)=O UWKAYLJWKGQEPM-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- JXTPJDDICSTXJX-UHFFFAOYSA-N n-Triacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC JXTPJDDICSTXJX-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QUMITRDILMWWBC-UHFFFAOYSA-N nitroterephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C([N+]([O-])=O)=C1 QUMITRDILMWWBC-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- AICOOMRHRUFYCM-ZRRPKQBOSA-N oxazine, 1 Chemical compound C([C@@H]1[C@H](C(C[C@]2(C)[C@@H]([C@H](C)N(C)C)[C@H](O)C[C@]21C)=O)CC1=CC2)C[C@H]1[C@@]1(C)[C@H]2N=C(C(C)C)OC1 AICOOMRHRUFYCM-ZRRPKQBOSA-N 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 235000021254 resistant starch Nutrition 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229940032094 squalane Drugs 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Description
【発明の詳細な説明】
この発明は、ガスクロマトグラフ用充てん剤に
関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a packing material for gas chromatography.
更に詳しくはこの発明は、ガスクロマトグラフ
用担体の表面にデンプンを固定相液体とともにコ
ートしたことからなるガスクロマトグラフ用充て
ん剤に関する。 More specifically, the present invention relates to a packing material for gas chromatographs, which is formed by coating the surface of a carrier for gas chromatographs with starch and a stationary phase liquid.
この発明によれば、特に香料の分析に適したガ
スクロマトグラフ用充てん剤が提供される。 According to the present invention, a packing material for gas chromatography is provided which is particularly suitable for analysis of fragrances.
一般的に、香料には多くの有機化合物が含有さ
れており、各成分の分離にはかなりの困難がつき
まとい、従来の充てん剤には満足すべきものがな
かつた。例えば、香料を分析するための充てん剤
として白色系ケイソウ土担体にフタル酸エステル
系のもののような耐熱性のある、比較的極性の大
きい固定相液体をコートしたものが用いられてい
た。ところがこのように担体表面を単に固定相液
体でコートしただけのものでは、ケイソウ土の表
面のシラノール基に基因して、ある特定成分のみ
が吸着されて分析ができなかつた。ケイソウ土担
体表面をジメチルジクロルシランやヘキサメチル
ジシラザンで処理して、シラノール基をつぶした
ものもあるが、これとても未反応の残存シラノー
ル基のためにこのような吸着に対してはたいした
効果をあげ得なかつた。この吸着された成分を脱
着させるのにリン酸を添加する方法があるが、リ
ン酸はアルデヒド基を有する成分と反応してしま
う等、脱着させようとする成分以外の成分に影響
を与えて、吸着分解がみられるという問題があつ
た。従つて、これまでは香料のような多成分を含
有する試料を分析するには何種類かの異つたカラ
ムで分析する方法でガスクロマトグラフイーに付
さなければ分析ができなかつた。 Generally, fragrances contain many organic compounds, and separation of each component is quite difficult, and conventional fillers have not been satisfactory. For example, a white diatomaceous earth carrier coated with a heat-resistant and relatively polar stationary phase liquid such as a phthalate ester has been used as a packing material for perfume analysis. However, when the carrier surface was simply coated with a stationary phase liquid, only certain components were adsorbed due to the silanol groups on the surface of diatomaceous earth, making analysis impossible. Some diatomaceous earth carrier surfaces are treated with dimethyldichlorosilane or hexamethyldisilazane to destroy the silanol groups, but these have very little effect on adsorption due to the unreacted residual silanol groups. I couldn't give up. There is a method of adding phosphoric acid to desorb this adsorbed component, but phosphoric acid reacts with components that have aldehyde groups, and affects components other than the component to be desorbed. There was a problem with adsorption and decomposition. Therefore, in the past, samples containing multiple components such as fragrances could only be analyzed using gas chromatography using several different columns.
この発明の発明者らは、上記のような点を解決
するために種々研究した結果、ガスクロマトグラ
フ用担体の表面に固定相液体とともに中性で耐熱
性の高いデンプンをコートすることにより、分析
対象である試料の全成分が吸着されずに分析する
ことができるのを見い出しこの発明に到達した。 The inventors of this invention conducted various studies to solve the above problems, and found that by coating the surface of a gas chromatography carrier with a neutral and highly heat-resistant starch together with a stationary phase liquid, it was possible to This invention was achieved by discovering that all components of a sample can be analyzed without being adsorbed.
この発明におけるデンプンとしては、何れの種
類でも用いることができるが、たとえばジヤガイ
モの塊茎、サツマイモの塊根、トウモロコシ、コ
ムギの種子、タピオカの根などから製造されたも
のが使用できる。 Any type of starch can be used in this invention, and for example, those produced from potato tubers, sweet potato tubers, corn, wheat seeds, tapioca roots, etc. can be used.
固定相液体としては、200℃以上の耐熱性（200
℃以上で分析に差しつかえない）を有し、かつ比
較的極性の大きいものが用いられる。極性につい
ては、ベンゼンを用いた場合のマクレイノルズ数
が90〜690であるものが好ましい。 As a stationary phase liquid, it has a heat resistance of 200℃ or higher (200℃
℃ or above) and relatively polar. Regarding polarity, it is preferable that the McReynolds number is 90 to 690 when benzene is used.
ここでマクレイノルズ数とは、ある試料液につ
いて被検充てん剤を充てんしてガスクロマトグラ
フイーに付した場合に得られるリテンシヨンイン
デツクス値から、スクアランを充てんした場合に
得られるリテンシヨンインデツクス値を差し引い
た値を意味し、充てん剤の特性を表わす数値であ
り、この値の高いことは固定相液体の極性度が増
すことを意味する。 Here, the McReynolds number is the retention index value obtained when a sample solution is filled with a test packing material and subjected to gas chromatography, and the retention index value obtained when the sample solution is filled with squalane. It is a numerical value that represents the characteristics of the packing material, and a higher value means that the polarity of the stationary phase liquid increases.
この発明の目的に好都合な固定相液体としては
サーモン―1000（Thermon―1000；フタル酸エ
ステル系の化合物で270℃でも使用可能）、カーボ
ワツクス20M（平均分子量20000のポリエチレン
グリコール）、FFAP〔平均分子量20000のポリエ
チレングリコールの末端基を２―ニトロテレフタ
ル酸としたもの〕等（いずれも信和化工(株)販売の
商品名）が挙げられる。 Stationary phase liquids suitable for the purpose of this invention include Thermon-1000 (a phthalate ester compound that can be used even at 270°C), Carbowax 20M (polyethylene glycol with an average molecular weight of 20,000), and FFAP (a polyethylene glycol with an average molecular weight of 20,000). polyethylene glycol whose end group is 2-nitroterephthalic acid] (all product names sold by Shinwa Kako Co., Ltd.).
担体としてはケイソウ土が適しており、白色系
のケイソウ土が好ましい。白色系ケイソウ土とし
ては、たとえばケイソウ土にアルカリ性融剤を加
えて加熱し、ケイソウ土の有する若干の酸性土や
活性点を減少せしめ、かつケイソウ土の色を白色
ならしめたものが用いられる。好ましい具体的市
販品としてはクロモソルブＷ（Chromosorb
Ｗ；Applied Science社（米国）製の商品名）や
ガスクロムＱ（Gas chrom Ｑ；Johns―
Manville社（米国）の商品名）が挙げられる。 Diatomaceous earth is suitable as a carrier, and white diatomaceous earth is preferred. The white type diatomaceous earth used is, for example, diatomaceous earth added with an alkaline flux and heated to reduce some of the acidic soil and active sites of the diatomaceous earth, and to make the diatomaceous earth white in color. A preferred specific commercial product is Chromosorb W (Chromosorb W).
W; trade name manufactured by Applied Science (USA)) and Gas chrom Q (Johns)
Manville (USA) product name).
ガスクロマトグラフ用担体にコートする上記二
つの成分の配合割合には好適な範囲が存在する。 There is a suitable range for the mixing ratio of the above two components to be coated on the carrier for gas chromatography.
デンプンは、固定相液体の種類や使用量にもよ
るが、少ないと所望の吸着防止・分離効果が得ら
れず、また多くなると担体表面に付着しにくくな
り、担体100重量部に対し約３〜８重量部の範囲
で使用されるのが好ましく、約５重量部の使用量
が最適である。 The amount of starch depends on the type and amount of stationary phase liquid used, but if it is too small, the desired adsorption prevention/separation effect cannot be obtained, and if it is too large, it becomes difficult to adhere to the surface of the carrier. Preferably, a range of 8 parts by weight is used, with an amount of about 5 parts by weight being optimal.
固定相液体は少ないと各試料成分の分離度が低
下し、また、多くなると各試料成分の溶出時間が
長くなるという問題が生ずる。担体100重量部に
対し約１〜25重量部の範囲で使用され、５重量部
近辺の使用量が最適である。 If the amount of stationary phase liquid is too small, the degree of separation of each sample component will decrease, and if it is too large, the elution time of each sample component will become longer. It is used in an amount of about 1 to 25 parts by weight based on 100 parts by weight of the carrier, and the optimum amount is around 5 parts by weight.
この発明のガスクロマトグラフ用充てん剤を製
造するには、通常の固体担液体表面のコーテイン
グ法が適用されるが、例えば前記２成分を溶媒に
溶解または分散し、これに担体の粉末を加え、溶
媒を蒸発させることにより製造される。 In order to produce the packing material for gas chromatography of the present invention, a usual method of coating the surface of a solid carrier liquid is applied. It is produced by evaporating.
次に実施例を挙げてこの発明を説明する。 Next, the present invention will be explained with reference to Examples.
実施例 １
フタル酸エステル系のThermon―1000 ５ｇと
バレイシヨデンプン５ｇをメタノール50mlに溶
解、分散させた後、これに白色系のケイソウ土担
体であるGas chromQ（80〜100メツシユの粒径
分布のもの）100ｇを加えて撹拌後、エバポレー
シヨン法でコートした。このようにして得られた
充てん剤を直径2.6mm、長さ４ｍのガラス製カラ
ムに充てんし、以下のような条件で香料の分析を
行つた。なおここで用いた香料は、分離および定
量性をチエツクするための標準試料である。Example 1 After dissolving and dispersing 5 g of phthalate ester-based Themon-1000 and 5 g of potato starch in 50 ml of methanol, a white diatomaceous earth carrier, Gas chromQ (with a particle size distribution of 80 to 100 mesh) was added to this. After adding 100g of the sample and stirring, it was coated using the evaporation method. The thus obtained packing material was filled into a glass column with a diameter of 2.6 mm and a length of 4 m, and the fragrance was analyzed under the following conditions. The fragrance used here is a standard sample for checking separation and quantitative properties.
試料：液体標準試料0.2μｌ
温度：130℃から230℃に昇温
昇温速度：３℃／min
キヤリヤーガス：N2
入口圧力：3.2Kg／cm2（230℃）
H2の流速：40ml／min
空気の流速：0.8l／min
検出器：FID
供給電圧：300V
レンジ：0.32V
感度：102
検出器温度：230℃
注入温度：230℃
チヤートスピード2.5mm／min
これによつて得られたクロマトグラムを第１図に
示す。Sample: Liquid standard sample 0.2μl Temperature: Increased temperature from 130℃ to 230℃ Temperature increase rate: 3℃/min Carrier gas: N 2 inlet pressure: 3.2Kg/cm 2 (230℃) H 2 flow rate: 40ml/min Air Flow rate: 0.8l/min Detector: FID Supply voltage: 300V Range: 0.32V Sensitivity: 10 2 Detector temperature: 230℃ Injection temperature: 230℃ Chart speed 2.5mm/min The chromatogram obtained by this Shown in Figure 1.
なお第１図における各ピークは次の化合物に対
応する。 In addition, each peak in FIG. 1 corresponds to the following compound.
ピーク 化合物
１…リモネン
２…ｐ―クレジルメチルエーテル
３…リナロオール
４…リナリルアセテート
５…ボルニルアセテート
６…シトロネリルアセテート
７…α―テルピネオール
８…シトロネロール
９…ゲラニオール
10…メチルイオノン
11…ローズ―ｐ
12…ラウリナール
13…リリアール
14…エチルシンナメート
15…オスミナール
16…ヘジオン
17…DEP
18…クメリン
19…ムスクアンブレツト
20…ベンジルベンゾエート
21…ベンジルサリチレート
22…ムスクケトン
比較例 １
デンプンを用いずにThermon―1000 ５ｇのみ
で実施例１と同様の担体を同様に処理することに
よりコートした。その他の条件は実施例１と全く
同一にして実施例１と同一試料の分析を行つた。
これにより得られた結果を第２図に示す。Peak Compound 1...Limonene 2...P-cresyl methyl ether 3...Linalool 4...Linalyl acetate 5...Bornyl acetate 6...Citronellyl acetate 7...α-Terpineol 8...Citronellol 9...Geraniol 10...Methyl ionone 11...Rose-p 12 …Laurinal 13…Lilyal 14…Ethyl cinnamate 15…Osminal 16…Hedion 17…DEP 18…Coumerin 19…Musk ambrella 20…Benzyl benzoate 21…Benzyl salicylate 22…Musk ketone Comparative example 1 Thermone without starch The same carrier as in Example 1 was coated with only 5 g of 1000 by the same treatment. The other conditions were completely the same as in Example 1, and the same sample as in Example 1 was analyzed.
The results obtained are shown in FIG.
実施例１と比較例を比較すると明らかなよう
に、デンプンを固定相液体とともにコートした充
てん剤は、デンプンを用いないものに較べると、
分離能において格段にすぐれている。 As is clear from comparing Example 1 and Comparative Example, the packing material coated with starch together with the stationary phase liquid has a higher
It has outstanding separation ability.
実施例 ２
Thermon―1000 ５ｇとバレイシヨデンプン５
ｇをメタノール50mlに溶解、分散させた後、これ
に白色系のケイソウ土担体であるクロモソルブＷ
（AW―DMCS）（80〜100メツシユの粒径分布の
もの）100ｇを加えて撹拌後、エバポレーシヨン
法でコートした。Example 2 Thermon-1000 5g and potato starch 5
After dissolving and dispersing g in 50 ml of methanol, Chromosolve W, a white diatomaceous earth carrier, was added to this.
(AW-DMCS) (with particle size distribution of 80 to 100 mesh) was added, stirred, and coated by evaporation.
このようにして得られた充てん剤を実施例１と
同様のカラムに充てんし、以下のような条件；
カラム温度：130℃→250℃（３℃／min）
キヤリヤーガス：N2，30ml／min
で実施例１で用いたのと異つた香料の標準試料を
分析した。これにより得られたクロマトグラムを
第３図に示す。 The packing material thus obtained was packed into the same column as in Example 1, and the conditions were as follows: Column temperature: 130°C → 250°C (3°C/min) Carrier gas: N 2 , 30ml/min A standard sample of a different fragrance than that used in Example 1 was analyzed. The chromatogram thus obtained is shown in FIG.
比較例 ２
バレイシヨデンプンを用いずにThermon―
1000 ５ｇのみで実施例２と同様のケイソウ土担
体を同様に処理することによりコートした。この
ようにして得られた充てん剤を用いて、その他は
実施例２と同様の条件で、実施例２と同一の試料
について分析を行つた。得られたクロマトグラム
を第４図に示す。Comparative Example 2 Thermon without potato starch
A diatomaceous earth support similar to Example 2 was coated with only 5 g of 1000 by the same treatment. Using the filler thus obtained, the same sample as in Example 2 was analyzed under the same conditions as in Example 2 except for the above. The obtained chromatogram is shown in FIG.
比較例 ３
0.5重量％のリン酸を加えること以外は比較例
２と同様にして分析を行つた。得られたクロマト
グラムを第５図に示す。Comparative Example 3 Analysis was conducted in the same manner as Comparative Example 2 except that 0.5% by weight of phosphoric acid was added. The obtained chromatogram is shown in FIG.
なお、第３〜４図中に記載した各記号は、それ
ぞれ下記の成分に対応する。 In addition, each symbol described in FIGS. 3 and 4 corresponds to the following components, respectively.
Ｃ：シトロネロール、Ma：ムスクアンブレツト
Ｇ：ゲラニオール、Bb：ベンジルベンゾエート
Ｒ：ローズ―Ｐ、Bs：ベンジルサリチレート
Ｌ：ラウリナール、Mk：ムスクケトン
Ｅ：オイゲノール
比較例２，３よりわかるように、無添加の充て
ん剤では特定の成分（オイゲノールとベンジルサ
リチレート）が吸着されてしまい（第４図参
照）、また0.5％のリン酸を添加した場合にはオイ
ノゲノールやベンジルサリチレート等は出てくる
が、シトロネロール、ゲラニオールおよびラウリ
ナールのピークはつぶれてしまう（第５図参
照）。C: citronellol, Ma: musk ambulette G: geraniol, Bb: benzyl benzoate R: Rose-P, Bs: benzyl salicylate L: laurinal, Mk: musk ketone E: eugenol As can be seen from Comparative Examples 2 and 3, no With the added filler, certain components (eugenol and benzyl salicylate) are adsorbed (see Figure 4), and when 0.5% phosphoric acid is added, eunogenol and benzyl salicylate are not released. However, the peaks of citronellol, geraniol, and laurinal are collapsed (see Figure 5).
これと比較して、この発明の充てん剤は、香料
の標準試料の各成分をうまく分離することができ
る（第３図参照）。 In comparison, the filler of the present invention is able to successfully separate the components of a standard sample of perfume (see Figure 3).
第１図および第３図はこの発明の充てん剤を用
いて香料の標準試料をガスクロマトグラフイーに
付した場合のクロマトグラムであり、第２図、第
４図および第５図は比較例で得られたクロマトグ
ラムである。
Figures 1 and 3 are chromatograms obtained when a standard sample of fragrance was subjected to gas chromatography using the packing material of the present invention, and Figures 2, 4, and 5 are chromatograms obtained in comparative examples. This is the chromatogram obtained.
Claims (1)
にデンプンを固定相液体とともにコートしたこと
からなるガスクロマトグラフ用充てん剤。1. A packing material for gas chromatographs consisting of a diatomaceous earth carrier coated with starch and a stationary phase liquid on the surface of a diatomaceous earth carrier for gas chromatographs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13090078A JPS5557147A (en) | 1978-10-23 | 1978-10-23 | Gas chromatograph filler |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13090078A JPS5557147A (en) | 1978-10-23 | 1978-10-23 | Gas chromatograph filler |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5557147A JPS5557147A (en) | 1980-04-26 |
| JPS6223256B2 true JPS6223256B2 (en) | 1987-05-22 |
Family
ID=15045337
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13090078A Granted JPS5557147A (en) | 1978-10-23 | 1978-10-23 | Gas chromatograph filler |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5557147A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3983299A (en) * | 1974-03-04 | 1976-09-28 | Purdue Research Foundation | Bonded carbohydrate stationary phases for chromatography |
-
1978
- 1978-10-23 JP JP13090078A patent/JPS5557147A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3983299A (en) * | 1974-03-04 | 1976-09-28 | Purdue Research Foundation | Bonded carbohydrate stationary phases for chromatography |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5557147A (en) | 1980-04-26 |
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