JPH0664039B2 - Simultaneous determination of glycyrrhizic acid and ehuedrins in crude drug combination preparations - Google Patents
Simultaneous determination of glycyrrhizic acid and ehuedrins in crude drug combination preparationsInfo
- Publication number
- JPH0664039B2 JPH0664039B2 JP19873585A JP19873585A JPH0664039B2 JP H0664039 B2 JPH0664039 B2 JP H0664039B2 JP 19873585 A JP19873585 A JP 19873585A JP 19873585 A JP19873585 A JP 19873585A JP H0664039 B2 JPH0664039 B2 JP H0664039B2
- Authority
- JP
- Japan
- Prior art keywords
- glycyrrhizic acid
- crude drug
- ehuedrins
- simultaneous determination
- drug combination
- 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
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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は生薬配合薬剤中のグリチルリチン酸（以下、Gl
yという）及びエフエドリン類の同時定量法、更に詳細
には、製剤に配合された甘草の成分であるGlyと麻黄の
成分であるノルエフエドリン、ｌ−エフエドリン、ｄ−
プソイドエフエドリン及びメチルエフエドリン（以下、
夫々NE、Ｅ、PE及びMEという）よりなるエフエドリン類
の同時定量法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention relates to glycyrrhizic acid (hereinafter, referred to as Gl
y) and a method for simultaneous determination of efedrins, and more specifically, Gly which is a component of licorice and norehuedrin, which is a component of mahuang, l-fuedrin, d-
Pseudo-Fedrin and Methyl-Fedrin (hereinafter,
And NE), E, PE and ME respectively).
従来、原生薬の甘草、麻黄又はこれを含む漢方エキス含
有製剤中のGly、NE、Ｅ、PE及びMEの定量は、Glyはメチ
ル化ガスクロマトグラフ法、HLC法等により、またNE、
Ｅ、PE及びMEはGC法、HLC法等により行なわれている。Conventionally, quantification of Gly, NE, E, PE and ME in a herbal medicine licorice, mahuang or a Chinese herb extract-containing preparation containing the same was carried out by Gly for methylated gas chromatography, HLC method, etc.
E, PE and ME are performed by the GC method, the HLC method and the like.
しかしながら、Glyは配糖体であり、一方エフエドリン
類はアルカロイドであつて両者全く異質であるため、こ
れらの方法は、それぞれの物質を別条件で分析しなくて
はならず、また条件により、他成分の妨害を除くための
多くの前処理を行なう必要がある等、操作上煩瑣なるを
免れえなかつた。However, since Gly is a glycoside, and ehuedrins are alkaloids and are completely different from each other, these methods require that each substance be analyzed under different conditions, and depending on the conditions, It was necessary to perform many pretreatments to remove the interference of the components, and it was inevitable that the operation was complicated.
〔問題点を解決するための手段〕 斯かる実状において、本発明者らは生薬配合薬剤中のGl
y及びエフエドリン類を迅速かつ高精度で定量できる方
法を提供せんと鋭意研究の結果、上記従来法の欠点がな
く、かつ種々の薬剤中のGly及びエフエドリン類の定量
が可能な定量法を見出し、本発明を完成した。[Means for Solving Problems] In such an actual situation, the present inventors have found that Gl
As a result of earnest research to provide a method capable of quantifying y and ephedrains quickly and with high accuracy, as a result, a quantification method that does not have the drawbacks of the above-mentioned conventional methods and is capable of quantifying Gly and ephedrains in various drugs, The present invention has been completed.
すなわち本発明は、生薬配合製剤を、次の及び、 酸性の極性溶媒 イオン対試薬 を含有する移動相を用いた逆相イオン対クロマトグラフ
に付し、溶離液ををUV検出器により分析することを特徴
とする生薬配合薬剤中のグリチルリチン酸及びエフエド
リン類の同時定量法を提供するものである。That is, the present invention is to subject a crude drug formulation to the following and reverse phase ion pair chromatography using a mobile phase containing an acidic polar solvent ion pair reagent, and analyze the eluent with a UV detector. The present invention provides a method for simultaneous determination of glycyrrhizic acid and efuedrins in a galenical combination drug characterized by the above.
本発明方法により分析する試料は、予めその一定量に移
動相を加え、水浴上で還流抽出を行ない、冷後振盪抽出
し、更に遠心分離する等して得られた抽出液として使用
するのが好ましい。斯くして得られた抽出液を逆相イオ
ン対クロマトグラフに付して分析を行なう。クロマト操
作は常法に従つて行なうことができる。The sample to be analyzed by the method of the present invention is used as an extract obtained by previously adding a mobile phase to a fixed amount thereof, performing reflux extraction on a water bath, extracting by shaking after cooling, and further centrifuging. preferable. The extract thus obtained is subjected to reverse phase ion pair chromatography for analysis. The chromatographic operation can be performed according to a conventional method.
カラムとしては、一般に用いられるシリカゲルをオクタ
デシルシランで化学処理させたものが使用され、例え
ば、TSK−GEL ODS−120T（東洋曹達社製）、NUCLEOSIL
−Ｃ１ ８〔マチエリー・ナゲル（Macherey−Nagel）社
製〕等のカラムが挙げられ、特にTSK−GEL ODS−120T
が好ましい。As the column, a commonly used silica gel chemically treated with octadecylsilane is used. For example, TSK-GEL ODS-120T (manufactured by Toyo Soda Co., Ltd.), NUCLEOSIL
-C 1 8 [Machieri-Nagel (Macherey-Nagel) Co.] and the like column can be mentioned, in particular TSK-GEL ODS-120T
Is preferred.
移動相としては、酸性の極性溶媒及びイオン対試薬を含
有するものが使用される。酸性の極性溶媒としては、ア
セトニトリルと水及び酸性物質を含む混液であつて例え
ば1N水酸化ナトリウム水溶液でpHを2.5〜5.0、特に好ま
しくはpHを3.0に調整したものが使用される。アセトニ
トリルと水及との混合比は30:70〜40:60となるようにす
るのが好ましい。酸性物質としては、例えば酒石酸が好
適に使用され、移動相の全組成中に0.015〜0.15重量％
となるように配合される。イオン対試薬としては、例え
ばラウリル硫酸ナトリウムが好適に使用され、移動相の
全組成中に0.1〜0.5重量％となるように配合される。ラ
ウリル硫酸ナトリウムは、麻黄の成分であるエフエドリ
ン類とイオン対を形成する、移動相として、アセトニト
リル−0.005M酒石酸溶液（pH3.0）−ラウリル硫酸ナト
リウムの混液を使用する場合、それらの混合比は35:65:
0.3（ｗ／ｖ％）が好ましい。A mobile phase containing an acidic polar solvent and an ion pair reagent is used. As the acidic polar solvent, a mixed solution containing acetonitrile, water and an acidic substance, which is adjusted to pH 2.5 to 5.0, particularly preferably pH 3.0 with a 1N sodium hydroxide aqueous solution, is used. The mixing ratio of acetonitrile and water is preferably 30:70 to 40:60. As the acidic substance, for example, tartaric acid is preferably used, and 0.015 to 0.15% by weight in the total composition of the mobile phase is used.
It is blended so that. As the ion pair reagent, for example, sodium lauryl sulfate is preferably used, and is mixed so as to be 0.1 to 0.5% by weight in the whole composition of the mobile phase. Sodium lauryl sulfate forms an ion pair with ehuedrins, which is a component of mahuang, and when a mixture of acetonitrile-0.005M tartaric acid solution (pH 3.0) -sodium lauryl sulfate is used as a mobile phase, their mixing ratio is 35:65:
0.3 (w / v%) is preferable.
溶離液中のGlyの検出は例えば254nmまたNE、PE、Ｅ、ME
等のアルカロイド類の検出は例えば210nmの紫外部吸収
により行なうことができる。UV検出は、２台の検出器を
用いる方法、あるいは１台の検出器を用い例えば254nm
でGlyを検出後例えば210nmに波長変更する方法等の方法
により行なうことができる。The detection of Gly in the eluent is, for example, 254 nm or NE, PE, E, ME.
Alkaloids such as can be detected by ultraviolet absorption at 210 nm, for example. For UV detection, use two detectors, or use one detector, eg 254 nm
After Gly is detected by the method described above, the wavelength can be changed to 210 nm, for example.
本発明に使用される移動相は、イオン対試薬がエフエド
リン類とイオン対を形成して溶出を調整し、またpHを酸
性とすることによりGlyの溶出を調整することができる
ため、Gly及びエフエドリン類を他の夾雑物より分離す
ることができる。The mobile phase used in the present invention is such that the ion-pairing reagent forms an ion-pair with ephedrains to regulate elution, and the pH can be adjusted to acidic to regulate elution of Gly. The species can be separated from other contaminants.
本発明のGly、NE、PE、Ｅ、MEの定量法は、それら含有
試料を分析用移動相にて還流・振盪抽出する程度の簡単
な操作後、抽出液を直接高速液体クロマトグラフに付す
ることができるため、従来法における前処理操作を必要
としない。また、GlyとNE、PE、Ｅ、MEは、別条件によ
つて分析するのが常識手段であつたが、２台の検出器
（１台の時は、途中で波長変更すれば良い）を用いるこ
とにより、試薬の迅速化が可能となつた。In the method for quantifying Gly, NE, PE, E, and ME of the present invention, the extracted liquid is directly subjected to high performance liquid chromatography after a simple operation such as refluxing and shaking extraction of the contained sample in the mobile phase for analysis. Therefore, the pretreatment operation in the conventional method is not required. In addition, Gly and NE, PE, E, and ME used to be analyzed under different conditions, but it is common practice to use two detectors (when using one detector, change the wavelength on the way). By using it, the reagents can be speeded up.
従つて本発明方法によれば、操作時間は１時間以内、精
度面においても、98％以上の信頼率で定量分析を行なう
ことが可能であり、本発明方法は製剤分析において非常
に有効なものである。Therefore, according to the method of the present invention, the operation time is within 1 hour, and in terms of accuracy, quantitative analysis can be performed with a reliability rate of 98% or more, and the method of the present invention is very effective in formulation analysis. Is.
次に実施例を挙げて説明する。 Next, examples will be described.
実施例１ 下記方法により漢方エキス配合顆粒剤中のグリチルリチ
ン酸及びエフエドリン類の同時定量を行なつた。Example 1 Simultaneous quantification of glycyrrhizic acid and efuedrin in a Chinese herb extract-containing granule was performed by the following method.
（１） 操作法 試料１日量を採取し、移動相30mlを加え水浴上で15分間
還流した後、10分間振盪抽出する。冷後、移動相にて正
確に50mlとし、遠心分離を行ない、上澄液を試料溶液と
する。これを次の条件で液体クロマトグラフに付す。(1) Operation method A daily sample is taken, 30 ml of mobile phase is added, the mixture is refluxed for 15 minutes on a water bath, and then shake-extracted for 10 minutes. After cooling, make exactly 50 ml in the mobile phase, centrifuge, and use the supernatant as the sample solution. This is subjected to liquid chromatography under the following conditions.
（２） 分離条件 カラム条件:TSK−GeL ODS−120T カラム管：内径4mm長さ25cm 移動相:pH3.0、0.005M酒石酸溶液−アセトニトリル−ラ
ウリル硫酸ナトリウム〔65:35:0.3（ｗ／ｖ％）〕 溶出速度:1.5ml／分 検出波長:UV254nm（グリチルリチン酸）UV210nm（エフ
エドリン類） （３） 使用装置 島津LC−3A型高速液体クロマトグラフ （４） 試 料 使用した試料は次の処方である。(2) Separation conditions Column conditions: TSK-GeL ODS-120T Column tube: Inner diameter 4 mm Length 25 cm Mobile phase: pH 3.0, 0.005 M tartaric acid solution-acetonitrile-sodium lauryl sulfate [65: 35: 0.3 (w / v% )] Elution rate: 1.5 ml / min Detection wavelength: UV254 nm (glycyrrhizic acid) UV210 nm (efedrins) (3) Equipment used Shimadzu LC-3A high performance liquid chromatograph (4) Samples The sample used was the following formulation. .
（処方） アセトアミノフエン 540（mg） サリチルアミド 600 リン酸ジヒドロコデイン 15 マレイン酸クロルフエニラミン 7.5 無水カフエイン 75 サツカリンナトリウム 20 トウモロコシデンプン 700 カルボキシメチルセルロースCa 300 精製白糖 1319.4 葛根湯加桔梗エキス＊ 1212 軽質無水ケイ酸 1200 安息香酸ナトリウム 12 ケイヒ油 3.7 乳 糖 3.7 ＊カツコン、カンゾウ、キキヨウ、ケイヒ、シヤクヤ
ク、シヨウキヨウ、タイソウ、マオウより製したエキス （５） 本発明方法により検出した各成分のピークを標
準溶液のピークと比較同定した結果を第１図及び第２図
に示す。(Prescription) Acetaminophen 540 (mg) Salicylamide 600 Dihydrocodeine phosphate 15 Chlorpheniramine maleate 7.5 Anhydrous cafeuin 75 Sodium satsukalin 20 Corn starch 700 Carboxymethylcellulose Ca 300 Purified sucrose 1319.4 Kakkonto Kakyo extract * 1212 Light anhydrous silica Acid 1200 Sodium benzoate 12 Keihi oil 3.7 Lactose 3.7 * Extracts made from katsukcon, licorice, kyoto, cinnamon, peony, citrus, tannin and maou (5) The peak of each component detected by the method of the present invention is the peak of the standard solution The results of comparison and identification with are shown in FIGS. 1 and 2.
実施例２ 下記方法により原生薬末配合錠剤中のグリチルリチン酸
及びエフエドリン類の同時定量を行なつた。Example 2 Simultaneous quantification of glycyrrhizic acid and ehuedrins in a crude drug powder-containing tablet was carried out by the following method.
（１） 操作法、分離条件及び使用装置 実施例１と同様。(1) Operating Method, Separation Conditions, and Equipment Used Same as in Example 1.
（２） 試 料 使用した試料は次の処方である。(2) Sample The sample used had the following formulation.
（処方） アセトアミノフエン 660（mg） サリチルアミド 800 マレイン酸クロルフエニラミン 7.5 dl−塩酸メチルエフエドリン 30 リン酸ジヒドロコデイン 15 無水カフエイン 150 ケイヒ末 300 シヨウキヨウ末 150 カンゾウ末 300 結晶セルロース 300 乳 糖 32.5 ヒドロキシプロピルセルロース 60 カルボキシメチルセルロースCa 150 タルク 30 ステアリン酸Mg 15 （３） 本発明方法により検出した各成分のピークを標
準溶液のピークと比較同定した結果を第３図及び第４図
に示す。(Prescription) Acetaminophen 660 (mg) Salicylamide 800 Chlorpheniramine maleate 7.5 dl-Methyl fueedrine hydrochloride 30 Dihydrocodeine phosphate 15 Anhydrous caffein 150 Keihi powder 300 Ginseng powder 300 Crystalline cellulose 300 Lactose 32.5 Hydroxy Propylcellulose 60 Carboxymethylcellulose Ca 150 Talc 30 Stearic acid Mg 15 (3) The results of comparative identification of the peaks of each component detected by the method of the present invention with the peaks of the standard solution are shown in FIGS. 3 and 4.
第１図及び第２図は漢方エキス配合顆粒剤中を本発明方
法で分析したときのクロマトグラムで、第１図は検出波
長をUV210nmに、第２図は検出波長をUV254nmに設定して
得たものである。 第３図及び第４図は原生薬末配合錠剤を本発明方法で分
析したときのクロマトグラムで、第３図は検出波長をUV
210nmに、第４図は検出波長をUV254nmに設定して得たも
のである。Figures 1 and 2 are chromatograms of the herb extract-containing granules analyzed by the method of the present invention. Figure 1 is obtained by setting the detection wavelength to UV210nm and Figure 2 is obtained by setting the detection wavelength to UV254nm. It is a thing. FIGS. 3 and 4 are chromatograms of the crude drug powder-blended tablets analyzed by the method of the present invention. FIG. 3 shows the detection wavelength of UV.
210 nm and Fig. 4 were obtained by setting the detection wavelength to UV254 nm.
Claims (1)
に付し、溶離液をUV検出器により分析することを特徴と
する生薬配合製剤中のグリチルリチン酸及びエフエドリ
ン類の同時定量法。1. A crude drug-containing drug, which is subjected to reverse phase ion pair chromatography using the following and a mobile phase containing an acidic polar solvent and an ion pair reagent, and the eluent is analyzed by a UV detector. A method for simultaneous determination of glycyrrhizic acid and efuedrins in a characteristic herbal medicine combination preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19873585A JPH0664039B2 (en) | 1985-09-09 | 1985-09-09 | Simultaneous determination of glycyrrhizic acid and ehuedrins in crude drug combination preparations |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19873585A JPH0664039B2 (en) | 1985-09-09 | 1985-09-09 | Simultaneous determination of glycyrrhizic acid and ehuedrins in crude drug combination preparations |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6258167A JPS6258167A (en) | 1987-03-13 |
| JPH0664039B2 true JPH0664039B2 (en) | 1994-08-22 |
Family
ID=16396110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19873585A Expired - Lifetime JPH0664039B2 (en) | 1985-09-09 | 1985-09-09 | Simultaneous determination of glycyrrhizic acid and ehuedrins in crude drug combination preparations |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0664039B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770885B (en) * | 2016-12-13 | 2018-10-26 | 佛山科学技术学院 | A method of indentification by TLC is carried out to licorice ingredient in a kind of reed mentioned in ancient books Huang powder for clearing lung-heat |
| CN107677740B (en) * | 2017-09-05 | 2021-03-12 | 广西壮族自治区食品药品检验所 | Multi-component quality control method of magnolia flower rhinitis pills |
| CN109580842B (en) * | 2019-01-17 | 2021-09-03 | 武汉生物化学制药有限公司 | Method for measuring dissolution rate of compound cholamine tablets |
-
1985
- 1985-09-09 JP JP19873585A patent/JPH0664039B2/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| ＪｏｕｒｎａｌｏｆＰｈａｒｍａｃｅｕｔｉｃａｌＳｃｉｅｎｃｅｓ，７１〔１０〕（１９８２）Ｐ．１１０８−１１１２ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6258167A (en) | 1987-03-13 |
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