JPH03186760A - Simultaneous analysis of benzoic acid, sorbic acid and dehydroacetic acid - Google Patents

Simultaneous analysis of benzoic acid, sorbic acid and dehydroacetic acid

Info

Publication number
JPH03186760A
JPH03186760A JP1326436A JP32643689A JPH03186760A JP H03186760 A JPH03186760 A JP H03186760A JP 1326436 A JP1326436 A JP 1326436A JP 32643689 A JP32643689 A JP 32643689A JP H03186760 A JPH03186760 A JP H03186760A
Authority
JP
Japan
Prior art keywords
acid
magnesium
dehydroacetic
mobile phase
benzoic acid
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.)
Pending
Application number
JP1326436A
Other languages
Japanese (ja)
Inventor
Hiroyuki Murakita
宏之 村北
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.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
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 Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP1326436A priority Critical patent/JPH03186760A/en
Publication of JPH03186760A publication Critical patent/JPH03186760A/en
Pending legal-status Critical Current

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

Abstract

PURPOSE:To separate three components; benzoic acid, sorbic acid and dehydroacetic acid without generating the tailing of peaks by using a mobile phase contg. a specific concn. of magnesium ions and analyzing a sample contg. the benzoic acid, sorbic acid and dehydroacetic acid with a column for reversed phase chromatograph. CONSTITUTION:The sample contg. the benzoic acid, sorbic acid and dehydroacetic acid is analyzed with the column 4 for reversed phase chromatograph by using the mobile phase contg. at least 0.05M magnesium ions, by which the benzoic acid, sorbic acid and dehydroacetic acid are simultaneously analyzed. The reason for confining the concn. of the magnesium ions to at least 0.05M lies in that if the concn. is below 0.05M the effect of the magnesium addition does not appear and the tailing of the peaks still arises. About <=0.3M is preferable as the upper limit of the magnesium ions in terms of dissolution to the mobile phase. The form of the magnesium to be added to the mobile phase is exemplified by, for example, magnesium acetate, etc., and the solvent to dissolve the magnesium salt is exemplified by, for example, a phosphoric acid buffer soln.

Description

【発明の詳細な説明】 0)産業上の利用分野 本発明は、王として食品添肌物に使用される安息香酸、
ノルビン酸、デヒドロ酢酸の同時分析法に圓する。
DETAILED DESCRIPTION OF THE INVENTION 0) Industrial Application Field The present invention is directed to benzoic acid, which is used as a food additive in skin products.
We are working on a simultaneous analysis method for norbic acid and dehydroacetic acid.

(ロ)従来技術 と9.に添加されておシ、かかる食品中の添加物に分析
することは品質管理の面から前景である。
(b) Prior art and 9. Analyzing such additives in food is a priority from a quality control perspective.

そこで、従来から・食品添加物中の上記三戎分七分析す
る試みがなされてか91次の条件で分析するのが知られ
ている。
Therefore, attempts have been made to perform the above-mentioned analysis of food additives under the following conditions.

カラム: shi m −pack CLC−OD8 
(6,0轄I、D×15備)(M3津製作所製) 移動相:20.mMリン酸ナナトリウム緩衝液PH4,
8)/メタノー/L’=4/1 移動相流量: 1v−1/創n 検出器:紫外分九光度計230 、、。
Column: shim-pack CLC-OD8
(6.0 unit I, D x 15 units) (manufactured by M3 Tsu Seisakusho) Mobile phase: 20. mM sodium phosphate buffer PH4,
8)/methanol/L'=4/1 Mobile phase flow rate: 1v-1/n Detector: Ultraviolet fraction 9 photometer 230.

(ハ)発明が解決しようとする課題 しかしながら、上記分析条件で分析すると・第3図に示
す如くデヒドロ酢酸のピータCに大きなテーリングが生
じていた。
(c) Problems to be Solved by the Invention However, when analyzed under the above analysis conditions, as shown in FIG. 3, large tailing occurred in the PETA C of dehydroacetic acid.

そのため、テーリング消失条件が各種検討されてきて$
−シ、その一つとして移動相υpH条件に低下させて(
PHk 3.5以下に丁;!3)分析する方法がある。
Therefore, various conditions for tailing disappearance have been investigated.
- One of them is to lower the mobile phase υ pH condition (
PHk below 3.5;! 3) There is a method of analysis.

この方法によれば、8g4図に示す如くピークのテーリ
ングはほぼ消失するが、ソルビン酸のピークbとデヒド
ロ酢酸のピークCが重なシ。
According to this method, peak tailing almost disappears as shown in Figure 8g4, but peak b of sorbic acid and peak C of dehydroacetic acid overlap.

三成分の分離が連成されない。なお、第3図。Separation of three components is not coupled. In addition, Fig. 3.

第4図中のaは安息香酸のピークを示す。In FIG. 4, a indicates the peak of benzoic acid.

そこで2本発明は、ピークのテーリングが生じない状態
で安息香酸、ンμビン酸、デヒドa酢酸の三成分の分離
に可能とする新規な分析法を提供することを目的とする
Therefore, it is an object of the present invention to provide a new analytical method that makes it possible to separate the three components of benzoic acid, mbic acid, and dehyde acetic acid without causing peak tailing.

に)課題χ解決するための手段 本件出願の発明者は、上記課題に解決するため鋭意検討
した結果、クロマトグラフカラムに試料に付丁ための移
動相中にマグネシウムイオン金所定量以上含有させるこ
とによりテーリングが生じない状態で三成分Q分離がで
きることχ見出し2本発明をなすに至ったのである。
B) Means for solving the problem χ As a result of intensive studies to solve the above problem, the inventor of the present application has decided to include more than a predetermined amount of magnesium ions and gold in the mobile phase for attaching the sample to the chromatography column. Accordingly, the present invention has been achieved based on the fact that three-component Q separation can be performed without tailing.

すなわち0本発明は、少なくともマグネシウムイオンが
0.05M含まれている移動相に用いて安息香酸、ン〜
ビン酸、デヒドロ酢酸含有試料に逆相クロマトグラフ用
カラムに付し、安息香酸、ンμビン酸、デヒドロ酢酸紫
同時分析することを特徴とする安息香酸、ソNビン酸、
デヒドロ酢酸の同時分析法である。
That is, in the present invention, benzoic acid,
Benzoic acid, so-N-binic acid, which is characterized in that a sample containing anic acid and dehydroacetic acid is subjected to a reversed-phase chromatography column for simultaneous purple analysis of benzoic acid, μ-binic acid, and dehydroacetic acid.
This is a simultaneous analysis method for dehydroacetic acid.

ここで、マグネシウムイオンの濃度を少なくとも0.0
5MとしたのHo、05 M未満だとマグネシウム添加
の効果が表われずピークのテーリングが依然として生じ
るからである。
Here, the concentration of magnesium ions is at least 0.0
This is because if the Ho content is less than 0.5 M, the effect of magnesium addition will not be apparent and peak tailing will still occur.

マグネシウムイオンの濃度の上限については特に規定さ
れないが、移動相中への溶解という観点からは0.3M
以下が好ましい。
The upper limit of the concentration of magnesium ions is not particularly specified, but from the viewpoint of dissolution in the mobile phase, it is 0.3M.
The following are preferred.

移動相に添加するマグネシウムの形態としては0例えば
酢酸マグネシウム、炭酸マグネシウム、硫酸マグネシウ
ムに挙げることができるがこれらに限定されない。
Examples of the form of magnesium added to the mobile phase include, but are not limited to, magnesium acetate, magnesium carbonate, and magnesium sulfate.

また、これらマグネシウム塩を溶かす溶媒としては2例
えばリン酸緩衝液を挙げることができ、溶かした溶液(
移動相)のpHtl、特に限定されないが、溶出位置の
関係からpH2,5〜3.5の範囲が好筐しい。
In addition, as a solvent for dissolving these magnesium salts, for example, phosphate buffer can be mentioned, and the dissolved solution (
Although the pH of the mobile phase (mobile phase) is not particularly limited, it is preferably in the range of pH 2.5 to 3.5 in view of the elution position.

なお、逆相クロマトグラフ用カラムとは、サンプルとの
間で疎水的相互作用を起こす基9例えば、オクタデシル
基、オクチμ基、トリメチル基をシリカゲμ担体に結合
した充てん剤が詰めらfしたカラムをいい1例えばOD
8カラム(島津製作所製)を挙げろことができる。
Note that a column for reversed-phase chromatography is a column packed with a packing material in which groups 9, such as octadecyl groups, octi-μ groups, and trimethyl groups, are bonded to a silicage μ carrier that causes hydrophobic interaction with the sample. For example, OD
8 column (manufactured by Shimadzu Corporation).

(ホ)作用 本発明では、移動相中のマグネシウムイオンがデヒドロ
酢酸とキレート生成することによジデヒドロ酢酸の水溶
性が増し、デヒドロ酢酸のピークのテーリングに防止す
ることができる。
(E) Effect In the present invention, the magnesium ion in the mobile phase forms a chelate with dehydroacetic acid, thereby increasing the water solubility of didehydroacetic acid and preventing tailing of the dehydroacetic acid peak.

(へ)実施例 第1図に本発明の方法紮実施するための装置χ示す。(f) Example FIG. 1 shows an apparatus for carrying out the method of the present invention.

1は移動相部、2は移動相送液ボンデ、3は試料インジ
ェクタ、4は逆相クロマトグラフ用カラム、5は検出器
χ各に表わす。
1 is a mobile phase unit, 2 is a mobile phase liquid feeding bonder, 3 is a sample injector, 4 is a column for reversed phase chromatography, and 5 is a detector χ.

かかる装置によう次の条件下分析rhりた。Such an apparatus was used for analysis under the following conditions.

移動相: 0.2M酢酢酸マグネシウムクシ酸で3゜2
にpHFA整した溶液/メタノール=3/l移動相流量
=IW4/mIm カラム: Shrm −paCk CLC−ODS (
6,01!I 1.D X 15検出棒:紫外分光九度
計 230 ttm分析結果を第2図に示すが、第2図
よシ木発明によればピークのテーリングがなく、シかも
三成分倉完全に分離できることがわかる。なお第2図中
Cはデヒドロ酢酸、aは安息香酸、bはソルビン酸のピ
ーク倉各々示す。
Mobile phase: 0.2M acetic acid magnesium citric acid at 3°2
pHFA-adjusted solution/methanol = 3/l Mobile phase flow rate = IW4/mIm Column: Shrm-paCk CLC-ODS (
6,01! I 1. D X 15 detection rod: Ultraviolet spectrometer 230 TTM analysis results are shown in Figure 2. Figure 2 shows that according to the invention, there is no tailing of peaks and that the three-component cluster can be completely separated. . In FIG. 2, C indicates the peaks of dehydroacetic acid, a indicates the peaks of benzoic acid, and b indicates the peaks of sorbic acid.

(ト)効果 本発明によれば、デヒドロ酢酸のテーリングがなく、三
成分の同時分析が可能となる。
(g) Effects According to the present invention, there is no tailing of dehydroacetic acid, and simultaneous analysis of three components becomes possible.

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

第1囚は1本発明に係る方法を実施するための装置図、
第2図は0本発明に係る方法にXシ三成分を分析した図
、第3図、第4図は従来法に工や三成分を分析したとき
の図である。 第 ■ 図 第3 図 α
The first prisoner is a diagram of an apparatus for carrying out the method according to the present invention,
FIG. 2 is a diagram showing the analysis of the three components using the method according to the present invention, and FIGS. 3 and 4 are diagrams showing the analysis of the three components using the conventional method. Figure ■ Figure 3 Figure α

Claims (1)

【特許請求の範囲】[Claims] 1、少なくともマグネシウムイオンが0.05M含まれ
ている移動相を用いて安息香酸、ソルビン酸、デヒドロ
酢酸含有試料を逆相クロマトグラフ用カラムに付し、安
息香酸・ソルビン酸、デヒドロ酢酸を同時分析すること
を特徴とする安息香酸、ソルビン酸、デヒドロ酢酸の同
時分析法。
1. Simultaneous analysis of benzoic acid, sorbic acid, and dehydroacetic acid by applying a sample containing benzoic acid, sorbic acid, and dehydroacetic acid to a reversed-phase chromatography column using a mobile phase containing at least 0.05M magnesium ions. A simultaneous analysis method for benzoic acid, sorbic acid, and dehydroacetic acid.
JP1326436A 1989-12-15 1989-12-15 Simultaneous analysis of benzoic acid, sorbic acid and dehydroacetic acid Pending JPH03186760A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1326436A JPH03186760A (en) 1989-12-15 1989-12-15 Simultaneous analysis of benzoic acid, sorbic acid and dehydroacetic acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1326436A JPH03186760A (en) 1989-12-15 1989-12-15 Simultaneous analysis of benzoic acid, sorbic acid and dehydroacetic acid

Publications (1)

Publication Number Publication Date
JPH03186760A true JPH03186760A (en) 1991-08-14

Family

ID=18187788

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1326436A Pending JPH03186760A (en) 1989-12-15 1989-12-15 Simultaneous analysis of benzoic acid, sorbic acid and dehydroacetic acid

Country Status (1)

Country Link
JP (1) JPH03186760A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102230926A (en) * 2011-06-22 2011-11-02 红云红河烟草(集团)有限责任公司 Method for measuring benzoic acid content in tobacco additive
CN104807912A (en) * 2015-05-13 2015-07-29 梧州市产品质量检验所 Method for detecting sorbic acid in food
CN108593827A (en) * 2018-04-18 2018-09-28 东北制药集团沈阳第制药有限公司 A kind of method of Determination of sorbic in detection levocarnitine oral solution
CN114778742A (en) * 2022-05-14 2022-07-22 重庆市食品药品检验检测研究院 Method for determining high-efficiency and high-precision dehydroacetic acid in puffed food

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102230926A (en) * 2011-06-22 2011-11-02 红云红河烟草(集团)有限责任公司 Method for measuring benzoic acid content in tobacco additive
CN104807912A (en) * 2015-05-13 2015-07-29 梧州市产品质量检验所 Method for detecting sorbic acid in food
CN108593827A (en) * 2018-04-18 2018-09-28 东北制药集团沈阳第制药有限公司 A kind of method of Determination of sorbic in detection levocarnitine oral solution
CN114778742A (en) * 2022-05-14 2022-07-22 重庆市食品药品检验检测研究院 Method for determining high-efficiency and high-precision dehydroacetic acid in puffed food

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