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JPH0820416B2 - Dye or pesticide analysis method - Google Patents
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JPH0820416B2 - Dye or pesticide analysis method - Google Patents

Dye or pesticide analysis method

Info

Publication number
JPH0820416B2
JPH0820416B2 JP5222766A JP22276693A JPH0820416B2 JP H0820416 B2 JPH0820416 B2 JP H0820416B2 JP 5222766 A JP5222766 A JP 5222766A JP 22276693 A JP22276693 A JP 22276693A JP H0820416 B2 JPH0820416 B2 JP H0820416B2
Authority
JP
Japan
Prior art keywords
dye
pesticide
organic solvent
electrophoresis
water
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 - Lifetime
Application number
JP5222766A
Other languages
Japanese (ja)
Other versions
JPH0755769A (en
Inventor
隆文 春見
義明 北村
茂広 葛原
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NORINSUISANSHO SHOKUHIN SOGO KENKYUSHOCHO
Original Assignee
NORINSUISANSHO SHOKUHIN SOGO KENKYUSHOCHO
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by NORINSUISANSHO SHOKUHIN SOGO KENKYUSHOCHO filed Critical NORINSUISANSHO SHOKUHIN SOGO KENKYUSHOCHO
Priority to JP5222766A priority Critical patent/JPH0820416B2/en
Publication of JPH0755769A publication Critical patent/JPH0755769A/en
Publication of JPH0820416B2 publication Critical patent/JPH0820416B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、色素または農薬の分析
方法に関し、詳しくは自由界面電気泳動法により色素ま
たは農薬を分析するにあたり、泳動媒体として有機溶媒
を用いることによって、効率よく分析する方法に関す
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for analyzing a dye or a pesticide, and more specifically, a method for efficiently analyzing a dye or a pesticide by using an organic solvent as an electrophoretic medium when the dye or the pesticide is analyzed by a free interface electrophoresis method. Regarding

【0002】[0002]

【従来の技術および発明が解決しようとする課題】キャ
ピラリー電気泳動法をはじめとする自由界面電気泳動法
は、溶液中における物質の電気的性質を利用した高性
能,高感度の分析方法として、生化学,有機化学,分析
化学等の分野で各種物質の分離、分析技術に用いられて
いる。
2. Description of the Related Art Free interface electrophoresis, including capillary electrophoresis, is used as a high-performance, high-sensitivity analytical method that utilizes the electrical properties of substances in a solution. It is used for separation and analysis technology of various substances in fields such as chemistry, organic chemistry, and analytical chemistry.

【0003】この自由界面電気泳動法では、従来より泳
動媒体(導電媒体)として水を基本とする緩衝液が用い
られている。しかし、この方法では、適用可能な試料
は水溶性のものに限られること、電流に伴うジュール
熱が多量に発生すること、分子量の小さな物質(イオ
ン)は、いわゆるコールラウシュ効果により、分離ピー
クに非対称的な広がりを生じ、感度や分離度が著しく劣
化すること、使用可能なpH領域が限られること、す
なわちpHが1以下の強酸性や13以上の強アルカリ性
の泳動媒体では、電気泳動の電流許容範囲を越えるた
め、このような条件下でのみイオン化する分子種には事
実上適用不能であること等の問題点を抱えていた。
In this free interface electrophoresis method, a buffer solution based on water has been used as an electrophoretic medium (conductive medium). However, in this method, applicable samples are limited to water-soluble ones, a large amount of Joule heat is generated with the current, and substances with small molecular weight (ions) are asymmetrical to the separation peak due to the so-called Colelauche effect. Current, the sensitivity and resolution are significantly deteriorated, and the usable pH range is limited. That is, in the case of a strongly acidic electrophoretic medium having a pH of 1 or less and a strongly alkaline electrophoretic medium having a pH of 13 or more, the electrophoretic current is allowed to flow. Since it exceeds the range, there is a problem in that it is practically inapplicable to molecular species that are ionized only under such conditions.

【0004】そこで、本発明者らは、従来より行われて
いる自由界面電気泳動法における上記課題を解決すべく
検討を重ね、泳動媒体として有機溶媒を使用することが
有効であることを見出し、本発明に到達したのである。
Therefore, the present inventors have conducted extensive studies to solve the above-mentioned problems in the conventional free interface electrophoresis method, and found that it is effective to use an organic solvent as a migration medium. The present invention has been reached.

【0005】[0005]

【課題を解決するための手段】本発明は、自由界面電気
泳動法により色素または農薬を分析するにあたり、泳動
媒体として有機溶媒を用いることを特徴とする色素また
は農薬の分析方法である。
The present invention is a method for analyzing a dye or a pesticide characterized by using an organic solvent as an electrophoretic medium when the dye or the pesticide is analyzed by a free interface electrophoresis method.

【0006】本発明が適用される物質は様々なものがあ
るが、特に色素や農薬(除草剤,殺虫剤,殺菌剤など)
等が好適で、とりわけ、各種食品中に含まれる色素や残
留農薬等の分析、定量に有効である。なお、本発明の方
法は、原理的にこれら物質の他に蛋白質,ペプチド,ア
ミノ酸,有機酸,天然色素,アルカロイド等の生化学物
質や糖類,酸アミド,合成抗菌剤などの分析、定量に利
用することが可能である。
There are various substances to which the present invention is applicable, but especially pigments and pesticides (herbicides, insecticides, fungicides, etc.)
Etc. are suitable, and are particularly effective for analysis and quantification of pigments and residual agricultural chemicals contained in various foods. The method of the present invention is used in principle for the analysis and quantification of biochemical substances such as proteins, peptides, amino acids, organic acids, natural pigments, alkaloids, sugars, acid amides, synthetic antibacterial agents, etc. in addition to these substances. It is possible to

【0007】泳動媒体として用いる有機溶媒は、例えば
メチルアルコール,エチルアルコール,アセトニトリ
ル,アセトン,二硫化炭素などがあり、これらを単独
で、あるいは強酸,強塩基を適宜加えて使用される。
The organic solvent used as the electrophoretic medium includes, for example, methyl alcohol, ethyl alcohol, acetonitrile, acetone, carbon disulfide and the like, and these are used alone or by adding a strong acid and a strong base appropriately.

【0008】有機溶媒を使用することにより、緩衝液イ
オンと試料イオンとの相互作用により生じるピーク感
度,分離度のコールラウシュ的劣化を完全に除くことが
できる。しかも、有機溶媒は通電量が水に比べて著しく
低く抑えられるため、ジュール熱によるピークの形状劣
化や熱拡散による広がりを防いで、分析感度を向上させ
ることができる。
By using the organic solvent, it is possible to completely eliminate the Kohllausch-like deterioration of the peak sensitivity and the resolution caused by the interaction between the buffer ions and the sample ions. In addition, since the amount of electricity applied to the organic solvent is significantly lower than that of water, it is possible to prevent deterioration of the peak shape due to Joule heat and spread due to thermal diffusion, and to improve the analytical sensitivity.

【0009】また、本発明で用いる有機溶媒は、その粘
性係数が水に比べて可なり低いため、水系では事実上実
現困難な低温(0〜10℃)で高速泳動を行うことが可
能である。なお、水の場合と異なり有機溶媒中ではプロ
トンの授受に伴う電荷の移動が起こらないため、水性の
試料液中でカチオンの分析を行うときは、メタンスルホ
ン酸等の強酸を、アニオンの分析を行うときは、水酸化
ナトリウム,ナトリウムエトキシド等の強塩基をそれぞ
れ用いて試料を予めイオン化することにより、水系緩衝
液中ではイオン化が不可能な物質をイオン化させて分析
することが可能である。
Further, since the organic solvent used in the present invention has a viscosity coefficient considerably lower than that of water, it is possible to carry out high-speed migration at a low temperature (0 to 10 ° C.) which is practically difficult to realize in an aqueous system. . Note that, unlike the case of water, charge transfer due to the transfer of protons does not occur in an organic solvent, so when analyzing cations in an aqueous sample solution, analyze strong acids such as methanesulfonic acid and anions. When performing, it is possible to ionize the substance that cannot be ionized in the aqueous buffer solution by previously ionizing the sample using strong bases such as sodium hydroxide and sodium ethoxide, and analyze it.

【0010】吸光度が小さく通常の分析が困難な金属カ
チオン(Ca2+,Fe2+ ,Ni2+ 等) や無機アニオン(SO
3 2-等)の分析を本発明の方法により行う場合、前者は
例えば4,2−(ピリジルアゾ)−レゾルシノール(PA
R) のような吸光性の強い金属指示薬とのキレート錯イ
オンの形で、また後者は例えばメチレンブルー,パラロ
ーザニリン等のイオン会合試薬とのイオン会合体の状態
で泳動させることにより、水中よりも安定かつ高感度な
分析が可能である。
Metal cations (Ca 2+ , Fe 2+ , Ni 2+ etc.) and inorganic anions (SO
3 2- etc.) is analyzed by the method of the present invention, the former is, for example, 4,2- (pyridylazo) -resorcinol (PA
R) in the form of a chelate complex ion with a highly light-absorbing metal indicator, and the latter in the state of an ion association with an ion association reagent such as methylene blue, pararosaniline, etc. Stable and highly sensitive analysis is possible.

【0011】また、炭化水素等のようにプロトン授受に
与かる官能基をもたない無電荷の非水溶性試料について
は、+電荷をもつテトラアルキルアンミンイオンとの疎
水的な結合を利用するにより、電気泳動的な分離ができ
る。
For an uncharged non-water-soluble sample having no functional group for proton transfer, such as hydrocarbon, the hydrophobic bond with the positively charged tetraalkylammine ion is used. , Electrophoretic separation is possible.

【0012】[0012]

【実施例】次に、本発明を実施例により詳しく説明す
る。 実施例1 カチオン系色素の分離、分析 下記の条件でキャピラリー電気泳動法を実施した。 キャピラリー:内径75μm,長さ50cmの溶融シリ
カ管 基本泳動媒体組成:10N−トリフルオロ酢酸を0.1%
含むアセトニトリル 供試試料:合成塩基性色素(フクシン,メチルバイオレ
ット,ブリリアントグリーン,メチレンブルー) アントシアニジン系色素(シアニジン,デルフィニジン
ペラルゴニジン) アニリン系脂溶性色素(クリソイジン,バターイエロー
* , オイルイエローOB* )(* は水に不溶性である。) 上記試料を最終濃度で25ppm になるように5N−トリ
フルオロ酢酸に溶解して用いた。 泳動条件:15℃,入口側電極+,出口側電極グラウン
ド、25KV,1.0μA 試料の検出:紫外部〜可視部吸光検出器
EXAMPLES Next, the present invention will be described in detail with reference to Examples. Example 1 Separation and Analysis of Cationic Dye Capillary electrophoresis was performed under the following conditions. Capillary: fused silica tube with inner diameter of 75 μm and length of 50 cm Basic electrophoretic medium composition: 0.1% of 10N-trifluoroacetic acid
Acetonitrile containing Samples: Synthetic basic dyes (fuchsin, methyl violet, brilliant green, methylene blue) Anthocyanidin dyes (cyanidine, delphinidin pelargonidin) Aniline fat-soluble dyes (chrysoidine, butter yellow)
* , Oil Yellow OB * ) ( * is insoluble in water.) The above sample was dissolved in 5N-trifluoroacetic acid to a final concentration of 25 ppm and used. Electrophoresis conditions: 15 ° C, inlet side electrode +, outlet side electrode ground, 25KV, 1.0μA Sample detection: UV-visible absorption detector

【0013】その結果、図1に示したように、供試した
すべてのカチオン系色素は20分以内に極めて効率よく
分離でき、ピークより算出した理論段数は、数万〜数十
万、検出感度は数十ppbであった。
As a result, as shown in FIG. 1, all the cationic dyes tested could be separated very efficiently within 20 minutes, the theoretical plate number calculated from the peak was tens of thousands to hundreds of thousands, and the detection sensitivity was Was several tens of ppb.

【0014】実施例2 アニオン系色素の分離、分析 下記の条件でキャピラリー電気泳動法を実施した。 キャピラリー:内径75μm,長さ50cmの溶融シリ
カ管 基本泳動媒体組成:6N−NaOHを0.1%含むアセト
ニトリルあるいはこれにテトラエチルアンモニウム塩を
数十ミリモル溶解させたもの 供試試料:酸性アゾ色素(アマランス,エリスロシン,
アルラレッド−AC)水不溶性の脂溶性アゾナフトール
色素(スダン−I,スダン−II,スダン−III) 上記試料を最終濃度で25ppm になるように6N−Na
OH/水に溶解して用いた。 泳動条件:15℃,入口側電極−,出口側電極グラウン
ド、25KV,1.0μA 試料の検出:紫外部〜可視部吸光検出器
Example 2 Separation and Analysis of Anionic Dye Capillary electrophoresis was carried out under the following conditions. Capillary: fused silica tube having an inner diameter of 75 μm and a length of 50 cm Basic electrophoretic medium composition: acetonitrile containing 0.1% of 6N-NaOH or tens of millimoles of tetraethylammonium salt dissolved Sample sample: acidic azo dye (Amaranth , Erythrosin,
Arla red-AC) Water-insoluble fat-soluble azonaphthol dyes (Sudan-I, Sudan-II, Sudan-III) 6N-Na was added to the above sample so that the final concentration was 25 ppm.
Used by dissolving in OH / water. Electrophoresis conditions: 15 ° C, inlet electrode-, outlet electrode ground, 25KV, 1.0μA Sample detection: UV-visible absorption detector

【0015】その結果、図2に示したように、供試した
すべてのアニオン系色素は30分以内に極めて効率よく
分離でき、実施例1と同様に理論段数は、数万〜数十
万、検出感度は数十ppbであった。
As a result, as shown in FIG. 2, all the anionic dyes tested could be separated very efficiently within 30 minutes, and the theoretical plate number was several tens to several hundreds of thousands as in Example 1. The detection sensitivity was several tens of ppb.

【0016】実施例3 無電荷,非水溶性成分の分離、分析 下記の条件でキャピラリー電気泳動法を実施した。 キャピラリー:内径75μm,長さ50cmの溶融シリ
カ管 基本泳動媒体組成:20mMテトラフルオロ酢酸,25
mMテトラエチルアンモニウムパークロレートを含むア
セトニトリル 供試試料:殺虫剤・殺菌剤(アシュラム* , イプロジオ
ン, ベンスリド,チラム,テトラエチルチラム, オキシ
ン銅) 脂溶性合成色素(バターイエロー* ,イエローOB*
スダン−I)(* は水に不溶性である。) 泳動条件:23℃,入口側電極+,出口側電極グラウン
ド、25KV 試料の検出:紫外部〜可視部吸光検出器
Example 3 Separation and analysis of uncharged and water-insoluble components Capillary electrophoresis was carried out under the following conditions. Capillary: fused silica tube with inner diameter of 75 μm and length of 50 cm Basic electrophoretic medium composition: 20 mM tetrafluoroacetic acid, 25
Acetonitrile containing mM tetraethylammonium perchlorate Samples: Insecticides / bactericides (Ashram * , Iprodione, Bencelide, Thiram, Tetraethyltyram, Oxin copper) Fat-soluble synthetic pigments (Butter Yellow * , Yellow OB * ,
Sudan-I) ( * is insoluble in water.) Electrophoresis conditions: 23 ° C, inlet side electrode +, outlet side electrode ground, 25KV Sample detection: UV-visible absorption detector

【0017】その結果、図3に示したように、電荷をも
たない9成分がすべて効率よく分離できた。また、理論
段数は、数万、検出感度は数十ppmであった。
As a result, as shown in FIG. 3, all 9 components having no electric charge could be efficiently separated. The theoretical plate number was tens of thousands, and the detection sensitivity was tens of ppm.

【0018】[0018]

【発明の効果】本発明の方法によれば、ピークの泳動速
度およびピーク面積の再現性は1〜2%の範囲に収ま
り、自由界面電気泳動法を食品等に含まれる色素や農薬
等の定量分析法として適用することが可能である。特
に、従来の水系泳動媒体を用いる電気泳動法では分離、
分析が不可能であった脂溶性合成色素について、高い理
論段数および再現性をもって分離、分析できることは画
期的なことである。
According to the method of the present invention, the migration rate of peaks and the reproducibility of peak areas are within the range of 1 to 2%, and free interface electrophoresis is used to quantify pigments and agricultural chemicals contained in foods. It can be applied as an analytical method. Especially, in the electrophoresis method using the conventional aqueous migration medium, separation,
It is epoch-making that lipophilic synthetic dyes that could not be analyzed can be separated and analyzed with a high theoretical plate number and reproducibility.

【図面の簡単な説明】[Brief description of drawings]

【図1】 カチオン系色素の分離、分析結果を示す。FIG. 1 shows the results of separation and analysis of cationic dyes.

【図2】 アニオン系色素の分離、分析結果を示す。FIG. 2 shows the results of separation and analysis of anionic dyes.

【図3】 無電荷、非水溶性成分の分離、分析結果を示
す。
FIG. 3 shows the results of separation and analysis of uncharged and water-insoluble components.

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 自由界面電気泳動法により色素または農
薬を分析するにあたり、泳動媒体として有機溶媒を用い
ることを特徴とする色素または農薬の分析方法。
1. A method for analyzing a dye or a pesticide, which comprises using an organic solvent as an electrophoretic medium when the dye or the pesticide is analyzed by a free interface electrophoresis method.
【請求項2】 色素または農薬が食品中に含まれるもの
である請求項1記載の方法。
2. The method according to claim 1, wherein the pigment or the agricultural chemical is contained in the food.
【請求項3】 有機溶媒がメチルアルコール,エチルア
ルコール,アセトニトリル,アセトンおよび二硫化炭素
の中から選ばれた物質を含むものである請求項1記載の
方法。
3. The method according to claim 1, wherein the organic solvent contains a substance selected from methyl alcohol, ethyl alcohol, acetonitrile, acetone and carbon disulfide.
【請求項4】 自由界面電気泳動法がキャピラリー電気
泳動法である請求項1記載の方法。
4. The method according to claim 1, wherein the free interface electrophoresis method is a capillary electrophoresis method.
JP5222766A 1993-08-17 1993-08-17 Dye or pesticide analysis method Expired - Lifetime JPH0820416B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5222766A JPH0820416B2 (en) 1993-08-17 1993-08-17 Dye or pesticide analysis method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5222766A JPH0820416B2 (en) 1993-08-17 1993-08-17 Dye or pesticide analysis method

Publications (2)

Publication Number Publication Date
JPH0755769A JPH0755769A (en) 1995-03-03
JPH0820416B2 true JPH0820416B2 (en) 1996-03-04

Family

ID=16787566

Family Applications (1)

Application Number Title Priority Date Filing Date
JP5222766A Expired - Lifetime JPH0820416B2 (en) 1993-08-17 1993-08-17 Dye or pesticide analysis method

Country Status (1)

Country Link
JP (1) JPH0820416B2 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE0201655D0 (en) * 2002-05-31 2002-05-31 Amersham Biosciences Ab A method of electrophoresis
US6939453B2 (en) * 2002-08-14 2005-09-06 Large Scale Proteomics Corporation Electrophoresis process using ionic liquids

Also Published As

Publication number Publication date
JPH0755769A (en) 1995-03-03

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