SU1594390A1 - Method of quantitative determination of aminophosphonic acids - Google Patents

Abstract

The invention relates to analytical chemistry and can be used to determine drugs, plant growth regulating agents, and the like. The purpose of the invention is to increase the accuracy, sensitivity and speed of the method. As a reagent, a solution of 0-phthalaldehyde and mercapto compounds is used in a molar ratio of from 1: 1 to 1:10. The reagent is injected into the sample to a concentration of 0-phthalic aldehyde 9 .10 -4 mol / l, PH 8-11, withstand the solution for 3 minutes and the optical density is determined at a wavelength of 340 nm, the value of which determines the content of aminophosphonic acid.

Description

The invention relates to the field of analytical chemistry, in particular to methods for the quantitative determination of amino-phosphonic acids, and can be used to determine drugs, means of controlling plant growth, etc.

The purpose of the invention is to increase the accuracy, sensitivity and speed of the method.

Example 1. Determination of 1-ami-o-ethylphosphonic acid at a ratio of o-phthalic aldehyde and mercaptoethanol 1: 2 and pH 10.0. .

0.25 ml of a solution of 1-aminoethylphosphonate 6-M concentration and 25 ml of a reagent, which is prepared by mixing 0.2 ml of a solution of o-phthalaldehyde with a concentration of 14.4 mg / ml in ethyl alcohol, 0.2 ml an ethanol solution of mercaptoethanol with a concentration of 15.6 ml / l and 12 ml of 0.1 M Goratnoy buffer with pH 10.0 (reagent is stable during the day) is placed in a spectrophotometer well and the optical density at 340 nm relatively diluted in two ways: for the reagent. Optical density.

measured after 3 minutes after mixing; no reagents, it is 0.185, which, at an extinction coefficient of 59000 ~ 300 cm, corresponds to the concentration of β-amknoethylphosphonic acid (6.25: o, zo) -10 m.

Example 2. Determination of 1-amyoethylphosphonic acid at a ratio of o-phthalic aldehyde Q and mercaptoethanol 1: 2 and pH 8.0.

0.25 ml of a solution of 1-aminoethylphosphonic acid concentration and 0.25 ml of a reagent prepared similarly to that described in Example 1, 15 about a pH of 0.1 M borate buffer 8.0, are placed in a spectrophotometer well and the optical density is measured as in example 1.

The optical density, measured 20 by 3 minutes after mixing the reagent-iroB, is 0.143, which, with an extinction of 4900t200 M cm-1, reflects the concentration of 1-aminoethylphosphonic acid (5.85tO, 25). 25 i Example 3. Determination of 1-amine-Noethylphosphonic acid at a 1: 2 ratio of o-phthalic aldehyde and mercaptoethanol and pH 11.0.

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0.25 ml of a solution of 1-aminoethylphosphonic acid with a concentration of 6–10 M and 0.25 ml of a reagent, which is prepared analogously to example 1, pH 0.1 M borate buffer 11.0, are mixed in a 35 spectrophotometer well and 3 min is measured as optical density as in 1F 1. The optical density is 0.177. with an extinction coefficient of 58001400 M cm –1, there is a corresponding concentration of 1-amino-methylphosphonic acid (6.10 ± 0.40).

Example 4. Determination of 1-amy-Noetstphosphonic acid using o-phthalic aldehyde and mercapto-45 ethanol at a ratio of 1: 2 and pH 6.0.

The initial concentration of H-aminoethyl | sponic acid. The reagent is prepared as described in Example 1, but the pH is 0.1 M borate buffer CQ 6.0. Optical density, determined analogously to example 1, is 0.035, which, with an extinction coefficient of 1100f250 M-CM-, corresponds to a concentration (6.36t1.18).

Example 5. Determination of 1-aminoethylphosphonic acid with o-phthalaldehyde and mercaptoethanol with a ratio of 1: 0.5 and pH 10.0.

The initial concentration of 1-.aminoethyl phosphonic acid is 6-10 M. The reagent is prepared by mixing 0.2 ml of the solution and o-phthalic aldehyde with a concentration of 14.4 mg / ml in ethanol, 0.5 ml of an ethanolic solution of mercaptoethanol, concentration 15, 6 ml / l and 12 ml of 0.1 M borate buffer with pH 10.0. The optical density, measured as in Example 1, is 0.045, which, with an extinction coefficient of 1500t f200 M cm, corresponds to the concentration of 1-aminoethylphosphonic acid (6.00f iO, 70) .10 - fM.

Example 6. Determination of 1-amoethylphosphonic acid with o-phthalic aldehyde and mercato-ethanol at a ratio of 1: 1 and pH 10, Initial concentration of 1-aminoethylphosphonic acid 6.0 10 M. Reagen is prepared by mixing 0.2 ml of o -phthalic aldehyde concentration of 14.4 mg / ml in ethyl alcohol 0.1 ml of ethanol solution of mercaptoethanol concentration of 15.6 ml / l and 12 ml of 0.1 M borate buffer with pH 10.0. The optical density, determined as described in Example 1, is 0.145, which, with an extinction coefficient of 5000t200 M cm, corresponds to a concentration (5.80 ± 0.25).

Example 7. Determination of 1-aminoethylphosphonic acid using o-phthalic aldehyde and mercaptoethanol at a ratio of 1:10 and pH 10.0.

The initial concentration of 1-aminoethylphosphonic acid is 6-10 M. The reagent is prepared by mixing 0.2 ml of a solution of o-phthalic aldehyde at a concentration of 14.4 mg / l in ethanol with 0.1 ml of an ethanolic solution of mercaptoethanol at a concentration of 156 ml / l and 12 ml of 0 , 1 M borate buffer. The optical density, measured as in Example 1, is 0.110. that at extinction coefficient 38001200 corresponds to the concentration of 1-amino-ethyl phosphonic acid (5.7910.32)

Example 8. Determination of 1-amino-3-methylbutylphosphonic acid at a 1: 2 ratio of o-phthalic aldehyde and mercaptoethanol and pH 10.0. The reagent is prepared as described in Example 1. The concentration of 1-amino-3-methylbutylphosphonic acid is 4-10 M. Optical density.

measured as in example 1, is 0.111, which, with the extinction coefficient M – cm, corresponds to a concentration of 1-amino-3-methylbutylphosphonic acid (3.80 iO, 25) 10 M,

Example 9, Determination of 1-amino-2-methylpropylphosphonic acid with o-phthalic aldehyde and mercaptoethanol (1: 2 ratio) at pH 10.0.

The reagent is prepared as described in Example 1. The concentration of 1-amino-2-methylpropylphosphonic acid. The optical density, measured as in Example 1, is 0.156, which is when the coefficient is; the extinction M cm corresponds to the concentration of 1-amino-2-methylproduct-phosphonic acid (5.80tO, 30).

Example 10. Determination of 3-aminopropylphosphonic acid using o-phthalic aldehyde and mercaptoethanol (1: 2 ratio) at pH 10.0.

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The reagent was prepared as in Example 1. The concentration of 3-aminopropylphosphonic acid 4. The optical density, measured as in Example 1, is that when the coefficient of extinction 46001300 corresponds to the concentration of 3-amino-n-opylphosphonic acid (3.90tO, 20).

Example 11. Determination of 1-aminoethylphosphonic acid using o-phthalic aldehyde and dithioretol at a molar ratio of 1: 2 and a pH of 10.0.

0.25 ml of 1-aminoethylphosphonic acid solution and 0.25 ml of reagent, which is prepared by mixing 0.2 ml of o-phthal solution

15

20

25

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The extinction ficient of 4500 + 250 M cm-corresponds to the concentration of 1-aminoethylphos background acid (6, OOiO, 30) 10-5M.

PRI me R 12. Determination of 1-amino-2-methylpropylphosphonic acid using o-phthalic aldehyde and dithiothreitol (1: 2 ratio) at pH 10.0.

The reagent is prepared and the optical density is measured as in Example 7. The concentration of 1-amino-2-methylpropylphosphonic acid is 6-10M. The measured optical density is 0.137, which at an extinction ratio corresponds to a concentration of 1-amino-2 methylpropylphosphonic acid ( 6.09

oh, zoo ..

Example 13. Determination of 3-aminopropylphosphonic acid. using o-phthalic aldehyde and dithiothreitol (1: 2 ratio) at pH 10.0.

The reagent is prepared and the optical density is measured as in Example 11. The initial concentration of 3-aminopropylphosphonic acid is 6-10 M. The measured optical density is 0.145, which at an extinction coefficient of 48001250 M cm

concentrations of 3-aminopropylphosphonic acid (6.02tO, 25) ..

Example 14. Determination of 1-amino-3-methylbutylphosphonic acid with o-phthalic aldehyde and dithiothreitol (1: 2 ratio) at pH 10.0.

The reagent is prepared and the optical density is measured as in Example 11. The initial concentration of 1-amino-3-methylbutylfoxonic acid is 4-10 M. The optical density is 0.080, which is when the extinction coefficient is Mccm

corresponds to convoy aldehyde concentrates 14.4 mg / ml dz 1-amino-3-methylbutylphospho- in ethanol, 0.2 ml ethanol- "°" ° acid (4.00-0.15).

Example 15. Determination of 1-aminoethylphosphonic acid with o-phthalic aldehyde and mercapto succinic acid at a ratio of 1: 2 and pH 10.0.

A solution of dithiothreitol with a concentration of 30.9 mg / ml and 12 ml of 0.1 M borate buffer with a pH of 10.0 (the reagent is stable for a day) is placed in a cell of the spectrophotometer and the optical density is measured at 340 nm. Since a stable chromophore is formed as a result, the measurement of the optical density can be carried out within one hour after mixing. The optical density measured 10 minutes after the mixing of the reagents is 0.135, which is equal to 594390

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15

20

25

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The extinction ficient of 4500 + 250 M cm- corresponds to the concentration of 1-aminoethylphosphonic acid (6, OOiO, 30) 10-5M.

PRI me R 12. Determination of 1-amino-2-methylpropylphosphonic acid using o-phthalic aldehyde and dithiothreitol (1: 2 ratio) at pH 10.0.

The reagent is prepared and the optical density is measured as in Example 7. The concentration of 1-amino-2-methylpropylphosphonic acid is 6-10 M. The measured optical density is 0.137, which at the extinction coefficient corresponds to the concentration of 1-amino-2-methylpropylphosphonic acid ( 6,

oh, zoo ..

Example 13. Determination of 3-aminopropylphosphonic acid. using o-phthalic aldehyde and dithiothreitol (1: 2 ratio) at pH 10.0.

The reagent is prepared and the optical density is measured as in Example 11. The initial concentration of 3-aminopropylphosphonic acid is 6-10 M 1. The measured optical density is 0.145, which at an extinction coefficient of 48001250 M cm

concentrations of 3-aminopropylphosphonic acid (6.02tO, 25) ..

Example 14. Determination of 1-amino-3-methylbutylphosphonic acid using o-phthalic aldehyde and dithiothreitol (1: 2 ratio) at pH 10.0.

The reagent is prepared and the optical density is measured as in Example 11. The initial concentration of 1-amino-3-methyl-butylfossonic acid is 4-10 M. The optical density is 0.080, which is when the extinction coefficient is Mcm

corresponds to the con "P ™ 1-amino-3-methylbutylphospho-" ° "° ° acid (4.00-0.15).

Example 15. Determination of 1-aminoethylphosphonic acid with o-phthalic aldehyde and mercapto succinic acid at a ratio of 1: 2 and pH 10.0.

0.25 ml of 1-aminoethylphosphonic acid solution and 0.25 ml of reagent, which is prepared by mixing 0.2 ml of o-phthalic aldehyde solution of 14.4 mg / ml in ethyl alcohol, 0.2 ml of mercaptoacidic acid solution 0.1 n. borate buffer in concentration

30.0 mg / ml and 5 MP 0.1 M borate buffer with pH 10.0. Then they proceed as described in Example 11. The optical density is 0.068, which, with the extinction coefficient A500i200 M, corresponds to the concentration of 1-amino-methylphosphonic acid (3.02tO, 15)

.

Example 16. Determination of 31-aminopropylphosphonic acid with o-phthalic aldehyde and macapto-succinic acid with a ratio of 1 PHNII 1: 2 and pH 10.0; The initial concentration of 3-aminopropylphosphonic acid H-M - M. Pea-- Nent is prepared and the optical density is measured as described in Example 15, the optical density is d, 078, which with an extinct ratio of 5000t250 M cm-corresponds to the concentration of 3-aminopropylphosphonic Acid (3.1210.16) 10-iM. Example 17. Determination of 1-amino-2-methylpropylphosphonic acid lots with ot-phthalic aldehyde and mercapto succinic acid at a ratio of 1: 2 and pH 10.0.

The initial concentration of 1-amino-21594390 .8

Example 18. Determination of 1-amino-3-methylbutylphosphonic acid with o-phthalic aldehyde and mercapto-succinic acid at a ratio of 1: 2 and pH 10.0.

The initial concentration is 1 amino 3-methylbutylphosphonic acid. The reagent is prepared and the optical density is measured as described in Example 15. The measured optical density is 0.075, which is

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extinction 4800 + 200 M cm - corresponds to the concentration of 1-amino-3-methyl-butylphosphonic acid (3.13tO, l5).

Formula

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1 | 1 methyl propyl phosphonic acid. Zo The reagent is prepared and the optical j iococ Tb is measured as described in Example 15. The measured optical density is 0.102, which is 4900t200 K-cm-corresponding to, the concentration of 1-amino-2-methylpropyphosphonic acids (4.16 ± 0.16).

the invention

The method of quantitative determination of aminophosphonic acids, which consists in the introduction of a reagent into the sample, spectrophotometry of the obtained solution and determination of the content. aminophosphonic acid in terms of optical density, that is, in order with. To increase the accuracy, sensitivity and expressivity of the method, o-phthalic is introduced into the sample as a reagent. aldehyde and mercapto compound with a molar ratio of from 1: 1 to 1:10 to an o-phthalaldehyde concentration of 9-10 M, the pH of the resulting solution is maintained with a buffer in the range of 8-11, the resulting solution is maintained for 3 minutes. at a wavelength of 340 to them.

The initial concentration is 1 amino 3-methylbutylphosphonic acid. The reagent is prepared and the optical density is measured as described in Example 15. The measured optical density is 0.075, which is equal to

extinction 4800 + 200 M cm - corresponds to the concentration of 1-amino-3-methyl-butylphosphonic acid (3.13tO, l5).

Formula

the invention

0

five

zo

The method of quantitative determination of aminophosphonic acids, which consists in the introduction of a reagent into the sample, spectrophotometry of the obtained solution and determination of the content. aminophosphonic acid in terms of optical density, that is, in order with. increase Accuracy, sensitivity and expressiveness of the method are introduced; o-phthalic is introduced into the sample as a reagent. the aldehyde and mercapto compound with a molar ratio of from 1: 1 to 1:10 to an o-phthalaldehyde concentration of 9-10 M, the pH of the resulting solution is maintained with a buffer in the range of 8-11, the resulting solution is maintained for 3 min. The wavelength is 340.

Claims (1)

Method of quantitative determination of aminophosphonic acids, which consists in introducing reagent into the sample, spectrophotometrically obtained solution and determining the content of aminophosphonic acid by optical density, which is different from o-phthalic is introduced into the sample. aldehyde and mercapto compound with a molar ratio of from 1: 1 to 1:10 to an o-phthalaldehyde concentration of 9-10 " ⁴ M; 340 nm wavelength.