CN112986423A - Content analysis method and application of aminoacetonitrile hydrochloride - Google Patents
Content analysis method and application of aminoacetonitrile hydrochloride Download PDFInfo
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Abstract
The invention relates to the technical field of chemical detection, in particular to a content analysis method of aminoacetonitrile hydrochloride and application thereof in the quality evaluation of aminoacetonitrile hydrochloride, wherein the content analysis method specifically comprises the steps of (1) respectively dissolving a sample to be detected and a standard sample with distilled water, catalyzing, deriving and extracting to obtain a sample solution and a standard sample solution; (2) and (3) carrying out high performance liquid chromatography analysis on the sample solution and the standard sample solution, taking a mixture of acetonitrile and an ammonium formate aqueous solution as a mobile phase, and calculating the content of the aminoacetonitrile hydrochloride in the sample to be detected through comparison with the standard sample. The method has strong specificity and good precision, is particularly suitable for quality evaluation and control of medical intermediates and organic synthetic raw materials, can meet the production requirements of high-quality medicines and other chemical products, and has important function and practical significance for ensuring the quality of final products.
Description
Technical Field
The invention relates to the technical field of chemical detection, and particularly relates to a content analysis method of aminoacetonitrile hydrochloride and application thereof.
Background
The aminoacetonitrile is also called 2-aminoacetonitrile, beta-aminoacetonitrile or glycinonitrile and the like, the storage form of the aminoacetonitrile is mostly hydrochloride, namely the aminoacetonitrile hydrochloride form, the aminoacetonitrile hydrochloride form is a chemical intermediate and a raw material with quite large dosage, is mainly applied to the preparation of glycine and ethylenediamine, novel anti-inflammatory drugs Iguratimod, timolol, plant regulator thidiazuron and the like, and has wide application in the pesticide and medicine fields.
Through examining relevant documents at home and abroad, the prior art detects that the content of aminoacetonitrile hydrochloride is mostly a chemical titration method, and a Flohard method is adopted to detect the content of chloride ions; there are also methods for detecting the content of perchloric acid by non-aqueous titration, but chemical titration methods have major disadvantages, such as high content of chloride ions in the titration process, which cannot be deducted if other chlorides are contained.
In addition, the gas phase method adopts alkali liquor to adjust the alkali liquor to be alkalescent for detection, but the water content is large, so that the adsorption of a chromatographic column is serious, and the repeatability, the accuracy and the like are poor. The liquid chromatography adopts more water phases and reverse phase columns, which easily leads the collapse of the chromatographic column to cause tailing, poor peak shape, poor stability and other results.
Therefore, it is necessary to provide a method for analyzing the content of aminoacetonitrile hydrochloride, which has a good chromatographic peak shape and a high reliability of the obtained result, and an application thereof.
Disclosure of Invention
The invention provides an aminoacetonitrile hydrochloride content analysis method and application thereof, aiming at the technical problems of poor accuracy, repeatability and stability of the existing aminoacetonitrile hydrochloride content analysis method.
In a first aspect, the invention provides a method for analyzing the content of aminoacetonitrile hydrochloride, which specifically comprises the following steps:
(1) dissolving a sample to be detected and a standard sample respectively with distilled water, catalyzing with an acetonitrile solution of triethylamine, derivatizing with an acetonitrile solution of phenyl isothiocyanate, extracting with n-hexane, and diluting with distilled water to obtain a sample solution and a standard sample solution;
(2) and (2) carrying out high performance liquid chromatography analysis on the sample solution and the standard sample solution obtained in the step (1), taking a mixture of acetonitrile and an ammonium formate aqueous solution as a mobile phase, and calculating the content of aminoacetonitrile hydrochloride in the sample to be detected through comparison with the standard sample.
Further, in the step (1), the volume ratio of triethylamine to acetonitrile in the acetonitrile solution of triethylamine is 10-20: 90-80, wherein the volume ratio of phenyl isothiocyanate to acetonitrile in the acetonitrile solution of phenyl isothiocyanate is 1: 40-80, wherein the derivatization time is 0.5-2 h, and the derivatization temperature is 20-40 ℃;
preferably, the volume ratio of triethylamine to acetonitrile is 14: 86, the volume ratio of phenyl isothiocyanate to acetonitrile is 1: 80, the derivatization time is 1h, and the derivatization temperature is 30 ℃.
Further, in the step (1), glutamic acid is used as an internal standard substance. Benzene isothiocyanate is used as a derivative, glutamic acid is used as an internal standard substance, and the derivative can be effectively and completely separated.
Further, in the step (2), a silica gel bonded C18 packed column is adopted, the column temperature is 30 ℃, the theoretical plate number is 5000, the detection wavelength is 230-265 nm, and the optimal detection wavelength is 254 nm. 254nm is the most stable UV absorption wavelength of aminoacetonitrile hydrochloride.
Further, in the step (2), the volume ratio of acetonitrile to an ammonium formate aqueous solution in the mobile phase is 3-15: 97-85, wherein the concentration of the ammonium formate aqueous solution is 10-100 mmol/L, and the flow velocity of the mobile phase is 0.8 mL/min;
preferably, the volume ratio of acetonitrile to aqueous ammonium formate solution is 5: 95, and the concentration of the ammonium formate aqueous solution is 80 mmol/L. The characteristics of different mobile phases with different polarities are utilized, the polarity of the mobile phases is changed by changing the proportion of the mobile phases, so that the distribution proportion of the sample among the mobile phases is influenced, and the separation result is achieved; by adopting the mobile phase, better separation effect can be obtained.
Further, in the step (2), after the instrument baseline is stabilized, samples are sequentially injected according to the sequence of the standard sample, the test sample and the standard sample, and the sample volume of each sample injection is 20 muL.
In a second aspect, the invention provides an application of the method for analyzing the content of aminoacetonitrile hydrochloride in the quality evaluation of aminoacetonitrile hydrochloride.
The beneficial effect of the invention is that,
the method for detecting the content of the aminoacetonitrile hydrochloride by the pre-column derivatization high performance liquid chromatography provided by the invention fills the blank in the field, the mass fraction of the aminoacetonitrile hydrochloride detected by the method is good in chromatographic peak shape, accurate in integral calculation result and good in repeatability, and the obtained result is high in reliability and is more accurate and timely; the method has strong specificity and good precision, is particularly suitable for quality evaluation and control of medical intermediates and organic synthetic raw materials, can meet the production requirements of high-quality medicines and other chemical products, and has important function and practical significance for ensuring the quality of final products.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a standard chromatogram of example 1;
FIG. 2 is a sample chromatogram in example 1;
FIG. 3 is a linear relationship diagram in example 4.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
EXAMPLE 1 aminoacetonitrile hydrochloride content analysis
The method comprises the following steps of purchasing raw materials to obtain 200 kg of aminoacetonitrile hydrochloride, and analyzing the content of the aminoacetonitrile hydrochloride, wherein the content analysis method comprises the following steps:
preparation of stock solution of standard sample
Accurately weighing 0.0524g (accurate to 0.0002g) of aminoacetonitrile hydrochloride standard sample and 0.0518g (accurate to 0.0002g) of glutamic acid in a 100mL volumetric flask, adding 80mL of secondary distilled water, dissolving by ultrasonic oscillation, cooling to room temperature, and diluting to scale with distilled water to obtain standard sample stock solution;
preparation of stock solution of sample
Accurately weighing 0.0530g (accurate to 0.0002g) of aminoacetonitrile hydrochloride sample and 0.0506g (accurate to 0.0002g) of glutamic acid in a 100mL volumetric flask, adding 80mL of secondary distilled water, dissolving by ultrasonic oscillation, cooling to room temperature, and diluting to scale with distilled water to obtain a sample stock solution;
preparation of acetonitrile solution of triethylamine
Accurately measuring 1.4mL of triethylamine solution, placing the triethylamine solution into a 10mL volumetric flask, measuring 8.6mL of acetonitrile, placing the acetonitrile into the volumetric flask, and shaking the solution uniformly for later use;
preparation of acetonitrile solution of phenyl isothiocyanate
Accurately transferring 25 mu L of phenyl isothiocyanate into a 5mL centrifuge tube by using a liquid transfer gun, adding 2mL of acetonitrile solution, and uniformly mixing for later use;
derivative treatment of standard sample and sample
Accurately measuring 200 mu L of standard sample and sample stock solution, respectively placing in a 1.5mL centrifuge tube, adding 100 mu L of acetonitrile solution of triethylamine and 100 mu L of acetonitrile solution of phenyl isothiocyanate, mixing uniformly, and standing at 30 ℃ for 1 h;
respectively adding 400 mu L of n-hexane into the centrifuge tube, shaking, standing for 10min, taking the lower layer solution, and filtering to obtain standard sample filtrate and sample filtrate;
test and data processing
The high performance liquid chromatograph adopted is an LC-20ATvp infusion pump and an SPD-20Avp ultraviolet detector of Shimadzu corporation, the chromatographic column is a silica gel bonded C18 packed column (Dalianglit Hypersil ODS 2150 mm x 4.6 μm, the column temperature is 30 ℃, the theoretical plate number is 5000), and the chromatographic column is prepared by mixing acetonitrile: and the volume ratio of 80mmol/L ammonium formate water is 5: 95 is a mobile phase, and the flow rate is 0.8 mL/min;
respectively taking 200 mu L of standard sample filtrate and sample filtrate, and respectively adding 800 mu L of secondary distilled water to obtain a standard sample solution and a sample solution;
after the machine self-checking is started, under the specified operation condition, after the baseline of the instrument is stabilized, a plurality of needle samples are continuously injected, the relative response value of each needle is calculated, after the relative response value of two adjacent needles is changed by less than 1.5%, the samples are sequentially injected according to the sequence of the standard samples, the sample samples and the standard samples, the volume of each sample injection is 20 mu L, the detection is carried out under the wavelength of 254nm, the chromatogram is shown in figures 1 and 2, 3.829min in the figure is an internal standard substance derivative, namely the chromatographic peak of a glutamic acid derivative, 6.608min is the chromatographic peak of the derivative of aminoacetonitrile hydrochloride, the impurity separation is complete, the peak shape is good, and the data shown in the following table 1 are obtained:
table 1 example 1 test results
Substitution formula
in the formula:
As-average value of the aminoacetonitrile hydrochloride derivative peak area in the standard;
Ar-average value of peak area of glutamic acid derivative as internal standard in the standard;
mrweighing the mass of the internal standard substance glutamic acid in the standard sample;
msweighing the mass of the aminoacetonitrile hydrochloride in the standard sample;
pi-the amount of aminoacetonitrile hydrochloride in the sample;
f is correction factor of aminoacetonitrile hydrochloride derivative and glutamic acid derivative in the standard sample;
Xi-mass fraction of aminoacetonitrile hydrochloride in the sample;
Ai-average value of the area of the peak of the aminoacetonitrile hydrochloride derivative in the sample;
A1-average value of peak area of glutamic acid derivative as internal standard in the sample;
miweighing the mass of the aminoacetonitrile hydrochloride in the sample;
m1weighing the mass of the internal standard substance glutamic acid in the sample;
f1-correction factors for aminoacetonitrile hydrochloride derivatives and glutamic acid derivatives in the sample;
the mass fraction of the sample calculated was 98.84%.
EXAMPLE 2 aminoacetonitrile hydrochloride content analysis
300 kg of aminoacetonitrile hydrochloride is obtained by purchasing raw materials, the content of the aminoacetonitrile hydrochloride is analyzed, and the content analysis method specifically comprises the following steps:
preparation of stock solution of standard sample
Accurately weighing 0.0538g (accurate to 0.0002g) of aminoacetonitrile hydrochloride standard sample and 0.0532g (accurate to 0.0002g) of glutamic acid in a 100mL volumetric flask, adding 80mL of secondary distilled water, dissolving by ultrasonic oscillation, cooling to room temperature, and diluting to scale with distilled water to obtain standard sample stock solution;
preparation of stock solution of sample
Accurately weighing 0.0521g (accurate to 0.0002g) of aminoacetonitrile hydrochloride and 0.0511g (accurate to 0.0002g) of glutamic acid in a 100mL volumetric flask, adding 80mL of secondary distilled water, dissolving by ultrasonic oscillation, cooling to room temperature, and diluting to scale with distilled water to obtain a sample stock solution;
preparing acetonitrile solution of triethylamine, preparing acetonitrile solution of phenyl isothiocyanate, and deriving standard sample and sample
The same as example 1;
test and data processing
The procedure was the same as in example 1, with complete separation of impurities and good peak shape, and the data shown in table 2 below were obtained:
table 2 example 2 test results
The content of the effective components in the sample is calculated according to the formula of the embodiment 1, and the mass fraction of the obtained sample is 98.92%.
EXAMPLE 3 repeatability test
Preparation of stock solution of standard sample
Accurately weighing 0.0513g (accurate to 0.0002g) of aminoacetonitrile hydrochloride standard sample and 0.0545g (accurate to 0.0002g) of glutamic acid into a 100mL volumetric flask, adding 80mL of secondary distilled water, dissolving by ultrasonic oscillation, cooling to room temperature, and diluting to scale with distilled water to obtain standard sample stock solution;
preparation of stock solution of sample
Accurately weighing 6 parts of a test sample containing 0.05g (accurate to 0.0002g) of aminoacetonitrile hydrochloride and 6 parts of glutamic acid 0.05g (accurate to 0.0002g) respectively, placing the test samples and the glutamic acid in a 100mL volumetric flask, adding 80mL of secondary distilled water, dissolving the test samples by ultrasonic oscillation, cooling the test samples to room temperature, and diluting the test samples to a scale with the distilled water to obtain 6 parts of a test sample stock solution;
preparing acetonitrile solution of triethylamine, preparing acetonitrile solution of phenyl isothiocyanate, and deriving standard sample and sample
The same as example 1;
test and data processing
The 6 samples were tested according to the method of example 1, and the impurities were completely separated and the peak shape was good, and the contents of the effective components of the samples were calculated according to the formula of example 1, and the data shown in the following table 3 were obtained. Therefore, the method has good repeatability of experimental results.
Table 3 example 3 test results
Example 4 Linear assay
Preparation of stock solution of sample
Accurately weighing 6 groups of aminoacetonitrile hydrochloride samples and glutamic acid according to the following table 4, respectively placing the samples into a 100mL volumetric flask, adding 80mL of secondary distilled water, ultrasonically oscillating for dissolution, cooling to room temperature, and diluting to a scale with distilled water to obtain 6 parts of sample stock solution, wherein the aminoacetonitrile hydrochloride concentrations are 215 mug/mL, 320 mug/mL, 445 mug/mL, 523 mug/mL, 608 mug/mL and 698 mug/mL respectively;
TABLE 4 amount of glutamic acid and each group of samples in the Linear assay
| |
1 | 2 | 3 | 4 | 5 | 6 |
| Test specimen | 0.0215g | 0.0320g | 0.0445g | 0.0523g | 0.0608g | 0.0698g |
| Glutamic acid | 0.0514g | 0.0520g | 0.0515g | 0.0528g | 0.0521g | 0.0518g |
Preparing acetonitrile solution of triethylamine, preparing acetonitrile solution of phenyl isothiocyanate, and deriving sample
The same as example 1;
test and data processing
The method of example 1 is used to detect 6 samples, the impurities are completely separated, the peak shape is good, as shown in fig. 3, the ratio of the peak area of the aminoacetonitrile hydrochloride to the peak area of the internal standard substance is used to perform linear regression on the ratio of the aminoacetonitrile hydrochloride to the sample amount of the internal standard substance in the sample, so as to obtain the following regression equation:
y＝0.8817x-0.0263，R2＝0.9997，
it can be seen that the aminoacetonitrile hydrochloride has good linear relationship in the range of 200-700 mug/mL.
Example 5 intermediate precision test
Preparation of stock solution of sample
Accurately weighing 0.05g (accurate to 0.0002g) of aminoacetonitrile hydrochloride and 0.05g (accurate to 0.0002g) of glutamic acid by 6 persons in different laboratories respectively, placing the samples and the glutamic acid in 100mL volumetric flasks respectively, adding 80mL of secondary distilled water, dissolving the solution by ultrasonic oscillation, cooling the solution to room temperature, and diluting the solution to a scale by using the distilled water to obtain 6 sample stock solutions;
preparing acetonitrile solution of triethylamine, preparing acetonitrile solution of phenyl isothiocyanate, and deriving sample
Different personnel respectively operate according to the method of the embodiment 1 in different laboratories;
test and data processing
The samples were tested by different personnel in different laboratories according to the method of example 1, and the data shown in the following table 5 were obtained. Therefore, the method has good intermediate precision in experimental results.
Table 5 example 5 test results
Example 6 stability test
Preparation of stock solution of sample
Accurately weighing 0.0528g (accurate to 0.0002g) of aminoacetonitrile hydrochloride and 0.0514g (accurate to 0.0002g) of glutamic acid, placing the samples and the glutamic acid into a 100mL volumetric flask, adding 80mL of secondary distilled water, dissolving the secondary distilled water by ultrasonic oscillation, cooling the solution to room temperature, and diluting the solution to a scale with distilled water to obtain a sample stock solution;
preparing acetonitrile solution of triethylamine, preparing acetonitrile solution of phenyl isothiocyanate, and deriving sample
The same as example 1;
test and data processing
After the preparation, the samples were tested according to the method of example 1 at 0, 1, 2, 4, 8, and 24 hours, respectively, the impurities were completely separated, the peak shape was good, and the contents of the effective components of the samples were calculated according to the formula of example 1, to obtain the data shown in table 6 below. Therefore, the method has good time stability of experimental results.
Table 6 example 6 test results
In conclusion, the method for analyzing the content of the aminoacetonitrile hydrochloride provided by the invention has high accuracy and good operability, and can be widely applied to the analysis and detection of the content of the aminoacetonitrile hydrochloride.
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. The method for analyzing the content of aminoacetonitrile hydrochloride is characterized by comprising the following steps:
(1) dissolving a sample to be detected and a standard sample respectively with distilled water, catalyzing with an acetonitrile solution of triethylamine, derivatizing with an acetonitrile solution of phenyl isothiocyanate, extracting with n-hexane, and diluting with distilled water to obtain a sample solution and a standard sample solution;
(2) and (2) carrying out high performance liquid chromatography analysis on the sample solution and the standard sample solution obtained in the step (1), taking a mixture of acetonitrile and an ammonium formate aqueous solution as a mobile phase, and calculating the content of aminoacetonitrile hydrochloride in the sample to be detected through comparison with the standard sample.
2. The method according to claim 1, wherein in the step (1), the volume ratio of triethylamine to acetonitrile in the acetonitrile solution of triethylamine is 10-20: 90-80, wherein the volume ratio of phenyl isothiocyanate to acetonitrile in the acetonitrile solution of phenyl isothiocyanate is 1: 40-80, the derivatization time is 0.5-2 h, and the derivatization temperature is 20-40 ℃.
3. The method of claim 2, wherein in step (1), the volume ratio of triethylamine to acetonitrile in the solution of triethylamine is 14: 86, the volume ratio of phenyl isothiocyanate to acetonitrile in the acetonitrile solution of phenyl isothiocyanate is 1: 80, the derivatization time is 1h, and the derivatization temperature is 30 ℃.
4. The method of claim 1, wherein in step (1), glutamic acid is used as an internal standard.
5. The method according to claim 1, wherein in the step (2), a silica gel bonded C18 packed column is used, the column temperature is 30 ℃, the theoretical plate number is 5000, and the detection wavelength is 230-265 nm.
6. The method of claim 5, wherein in step (2), the detection wavelength is 254 nm.
7. The method of claim 1, wherein in step (2), the volume ratio of acetonitrile to the aqueous ammonium formate solution in the mobile phase is 3-15: 97-85, wherein the concentration of the ammonium formate aqueous solution is 10-100 mmol/L, and the flow velocity of the mobile phase is 0.8 mL/min.
8. The method of claim 7, wherein in step (2), the volume ratio of acetonitrile to aqueous ammonium formate solution in the mobile phase is from 5: 95, and the concentration of the ammonium formate aqueous solution is 80 mmol/L.
9. The method according to claim 1, wherein in the step (2), after the instrument baseline is stabilized, the samples are sequentially injected according to the sequence of standard sample, test sample and standard sample, and the sample volume of each injection is 20 μ L.
10. Use of the method according to any one of claims 1 to 9 in the quality evaluation of aminoacetonitrile hydrochloride.
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| JP2003176261A (en) * | 2001-10-05 | 2003-06-24 | Showa Denko Kk | Method for producing aminoacetonitrile and glycine derivative |
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| WO2013170308A1 (en) * | 2012-05-17 | 2013-11-21 | Commonwealth Scientific And Industrial Research Organisation | Hydrogen cyanide-based polymer surface coatings and hydrogels |
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| JP2003176261A (en) * | 2001-10-05 | 2003-06-24 | Showa Denko Kk | Method for producing aminoacetonitrile and glycine derivative |
| WO2013170308A1 (en) * | 2012-05-17 | 2013-11-21 | Commonwealth Scientific And Industrial Research Organisation | Hydrogen cyanide-based polymer surface coatings and hydrogels |
| CN103214381A (en) * | 2013-05-14 | 2013-07-24 | 张家港威胜生物医药有限公司 | Method for preparing 2-hydroxyl-2-(4-methoxylphenyl) ethylamine hydrochloride |
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