CN109298122B - Method for detecting purity of R-glyceraldehyde acetonide finished product - Google Patents
Method for detecting purity of R-glyceraldehyde acetonide finished product Download PDFInfo
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Abstract
The invention provides a method for detecting the purity of a finished product of R-glyceraldehyde acetonide, which comprises the following steps: 1) adding an organic solvent into the finished product of the R-glyceraldehyde acetonide for dissolving to obtain a liquid to be detected; 2) adding an organic solvent into an R-glyceraldehyde acetonide standard substance and an S-glyceraldehyde acetonide standard substance for dissolving to obtain a standard solution; 3) and respectively detecting the liquid to be detected and the standard solution by adopting GC-FID, comparing retention time according to the measured value of the standard solution for qualitative determination, determining the R-glyceraldehyde acetonide component and the S-glyceraldehyde acetonide component in the liquid to be detected, and determining the relative content of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide in the liquid to be detected by adopting a peak area normalization method. The method for detecting the purity of the R-glyceraldehyde acetonide finished product can realize the complete separation of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide, and has the advantages of good precision and accuracy and accurate result.
Description
Technical Field
The invention belongs to the technical field of organic compound purity detection, relates to a method for detecting the purity of a finished product of R-glyceraldehyde acetonide, and particularly relates to a method for detecting the contents of R-glyceraldehyde acetonide and S-glyceraldehyde acetonide in the finished product of R-glyceraldehyde acetonide.
Background
The chemical name of the R-glyceraldehyde acetonide is (R) - (+) -2, 2-dimethyl-1, 3-dioxo-4-aldehyde pentane, which is a key intermediate for synthesizing chiral drugs and has good industrial application value.
At present, isomerization reaction occurs in the process of preparing R-glyceraldehyde acetonide finished products to generate a small amount of S-glyceraldehyde acetonide, and the existing method for detecting the purity of the R-glyceraldehyde acetonide finished products is gas chromatography, and a common polar, medium polar or non-polar chromatographic column cannot separate chiral isomers, so that the detection result of the purity of the R-glyceraldehyde acetonide finished products is inaccurate. When R-glyceraldehyde acetonide containing S-glyceraldehyde acetonide is further prepared into a downstream chiral compound, isomers of the R-glyceraldehyde acetonide containing S-glyceraldehyde acetonide are difficult to separate, and the quality of the chiral drug is finally influenced. Therefore, a simple, convenient and accurate detection method is established for determining the purity of the R-glyceraldehyde acetonide finished product, particularly for effectively detecting the content of S-glyceraldehyde acetonide, and the method has important significance for monitoring the quality of the R-glyceraldehyde acetonide.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention is directed to a method for detecting the purity of R-glyceraldehyde acetonide product, which can effectively detect the contents of R-glyceraldehyde acetonide and S-glyceraldehyde acetonide in the R-glyceraldehyde acetonide product, thereby effectively controlling the quality of the purity of R-glyceraldehyde acetonide in the R-glyceraldehyde acetonide product.
In order to achieve the above objects and other related objects, the present invention provides a method for detecting the purity of a finished product of R-glyceraldehyde acetonide, comprising the following steps:
1) sample pretreatment: adding an organic solvent into the finished product of the R-glyceraldehyde acetonide for dissolving to obtain a liquid to be detected;
2) preparation of a standard solution: adding an organic solvent into an R-glyceraldehyde acetonide standard substance and an S-glyceraldehyde acetonide standard substance for dissolving to obtain a standard solution;
3) sample detection: respectively detecting the liquid to be detected in the step 1) and the standard solution in the step 2) by adopting a gas chromatography-flame ionization detector method (GC-FID), comparing and retaining time according to the measured value of the standard solution for qualitative determination, determining the components of R-glyceraldehyde acetonide and S-glyceraldehyde acetonide in the liquid to be detected, and determining the relative contents of the components of R-glyceraldehyde acetonide and S-glyceraldehyde acetonide in the liquid to be detected by adopting a peak area normalization method.
Preferably, in step 1), R-glyceraldehyde acetonide finished product contains R-glyceraldehyde acetonide and S-glyceraldehyde acetonide. The CAS number of the R-glyceraldehyde acetonide is 15186-48-8. The CAS number of the S-glyceraldehyde acetonide is 22323-80-4.
Preferably, in the step 1), the ratio of the mass g of the added R-glyceraldehyde acetonide finished product to the volume ml of the added organic solvent is 2-3: 50.
Preferably, in the step 2), the R-glyceraldehyde acetonide standard is a standard product with the content of R-glyceraldehyde acetonide being more than or equal to 98.0% and produced by Kyoho high-tech materials, Inc.
Preferably, in step 2), the S-glyceraldehyde acetonide standard is produced by Jiuding chemical (Shanghai) science and technology, and the standard further comprises R-glyceraldehyde acetonide.
Preferably, in the step 2), the ratio of the mass g of the added R-glyceraldehyde acetonide standard substance to the volume ml of the added organic solvent is 2-3: 50.
Preferably, in the step 2), the ratio of the mass g of the S-glyceraldehyde acetonide standard added to the volume ml of the organic solvent added is 2-3: 50.
Preferably, in step 1) or 2), the organic solvent is selected from one of acetone, dichloromethane, ethyl acetate, toluene and acetonitrile.
Preferably, in the step 3), the chromatographic column adopted by the GC-FID method is a chemically bonded beta-cyclodextrin stationary phase filler chromatographic column (Coating CP chromatography oil Dex CB column), the length of the chromatographic column is 25m, the inner diameter is 0.25mm, and the thickness of the stationary phase membrane is 0.39 μm.
Preferably, in the step 3), the GC-FID method is performed in a sample amount of 0.1 to 1.0. mu.L. More preferably, the GC-FID method uses a sample size of 0.2. mu.L.
Preferably, in the step 3), the carrier gas adopted by the GC-FID method is high-purity helium, and the purity of the carrier gas is more than or equal to 99.999%.
Preferably, in step 3), the GC-FID method uses a carrier gas flow rate of 2.0-4.0 mL/min. More preferably, the GC-FID process employs a carrier gas flow rate of 3.0 mL/min.
Preferably, in the step 3), the sampling mode adopted by the GC-FID method is split sampling, and the split ratio is 50: 1.
Preferably, in the step 3), the injection port temperature adopted by the GC-FID method is 250-300 ℃. More preferably, the GC-FID method employs a sample inlet temperature of 280 ℃.
Preferably, in step 3), the detector used in the GC-FID method is a flame ionization detector (hydrogen flame detector, FID).
Preferably, in the step 3), the detector temperature adopted by the GC-FID method is 250-300 ℃. More preferably, the GC-FID method employs a detector temperature of 300 ℃.
Preferably, in the step 3), the temperature rising program adopted by the GC-FID method is as follows: the initial temperature is 40-70 deg.C, and is maintained for 1-3min, and the temperature is increased to 200 deg.C at a rate of 5-15 deg.C/min, and is maintained for 10-30 min.
More preferably, the GC-FID method adopts a temperature rising program comprising the following steps: the initial temperature was 50 ℃ for 2min, and the temperature was raised to 200 ℃ at a rate of 10 ℃/min for 13 min.
Preferably, in step 3), the peak area normalization method is: and (3) detecting the finished product sample of the R-glyceraldehyde acetonide by GC-FID, respectively calculating the chromatographic peak areas of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide, and calculating the sum of the areas of the chromatographic peaks in the finished product of the R-glyceraldehyde acetonide to obtain the total chromatographic peak area. Then, the chromatographic peak area of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide is divided by the total chromatographic peak area to obtain the percentage of the chromatographic peak area of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide to the total chromatographic peak area, which is the relative content of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide.
Preferably, in the step 3), the peak area normalization method is calculated according to formula (1), where formula (1) is: (Ai/Σ Ai) × 100%, where wi is the relative content of R-glyceraldehyde acetonide or the relative content of S-glyceraldehyde acetonide in the finished R-glyceraldehyde acetonide sample; ai is the chromatographic peak area of R-glyceraldehyde acetonide or the chromatographic peak area of S-glyceraldehyde acetonide in the R-glyceraldehyde acetonide finished product sample; sigma Ai is the total chromatographic peak area in the R-glyceraldehyde acetonide finished product sample.
As mentioned above, the method for detecting the purity of the R-glyceraldehyde acetonide finished product provided by the invention adopts a gas chromatography-flame ionization detector method (GC-FID) to detect the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide in the R-glyceraldehyde acetonide finished product, can realize the complete separation of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide as chiral isomers through the optimal detection conditions, makes up for the defects of the existing detection method of the product, and has good precision and accuracy and accurate result. The detection method adopts a peak area normalization method for quantification, and is simple in quantification method and good in repeatability.
Drawings
FIG. 1 shows a gas chromatogram for the measurement of R-glyceraldehyde acetonide as a finished product in the present invention, wherein a is S-glyceraldehyde acetonide and b is R-glyceraldehyde acetonide.
FIG. 2 shows a gas chromatogram for the measurement of S-glyceraldehyde acetonide standard in the present invention, wherein a is S-glyceraldehyde acetonide and b is R-glyceraldehyde acetonide.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It should be understood that the processing equipment or devices not specifically mentioned in the following examples are conventional in the art; all pressure values and ranges refer to relative pressures.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
The reagents and equipment used in the following examples are as follows:
1. reagent
R-Glycerol Acetal acetonide finished product (commercially available); r-glyceraldehyde acetonide standard (R-glyceraldehyde acetonide content is more than or equal to 98.0%, Kyoto Ming dynasty high and new technology materials Co., Ltd.); s-glyceraldehyde acetonide standard (containing R-glyceraldehyde acetonide, Jiuding chemical (Shanghai) science and technology Co., Ltd.); acetone, dichloromethane, ethyl acetate, toluene (analytical purity, chemical reagents of national drug group, ltd.); acetonitrile (chromatographically pure, Merck, Germany).
2. Instrument for measuring the position of a moving object
An Agilent model 7890A gas chromatograph (Agilent, usa) equipped with a flame ionization detector; agilent beta-cyclodextrin stationary phase packed chromatography column (25 m. times.0.25 mm, 0.39 μm) (Agilent Inc., USA).
Example 1
1. Sample pretreatment
And adding the finished product of the R-glyceraldehyde acetonide into an organic solvent for dissolving to obtain a liquid to be detected. Wherein the organic solvent is selected from one of acetone, dichloromethane, ethyl acetate, toluene and acetonitrile. The ratio of the mass g of the added R-glyceraldehyde acetonide finished product to the volume ml of the added organic solvent is 2-3: 50.
2. Preparation of Standard solutions
And respectively taking the R-glyceraldehyde acetonide standard substance and the S-glyceraldehyde acetonide standard substance, and adding an organic solvent to dissolve the R-glyceraldehyde acetonide standard substance and the S-glyceraldehyde acetonide standard substance to obtain standard solutions. Wherein the ratio of the mass g of the R-glyceraldehyde acetonide standard substance to the volume ml of the organic solvent is 2-3: 50. The ratio of the mass g of the S-glyceraldehyde acetonide standard substance to the volume ml of the organic solvent is 2-3: 50. The organic solvent is selected from one of acetone, dichloromethane, ethyl acetate, toluene and acetonitrile.
3. Measurement of
And (3) detecting the liquid to be detected prepared in the step (1) and the standard solution prepared in the step (2) by adopting GC-FID, comparing retention time according to the measured value of the standard solution for qualitative determination, determining the R-glyceraldehyde acetonide component and the S-glyceraldehyde acetonide component in the R-glyceraldehyde acetonide finished product, and determining the relative contents of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide in the R-glyceraldehyde acetonide finished product by adopting a peak area normalization method.
In specific determination, the detection conditions of the GC-FID method are as follows: the chromatographic column is a chemically bonded beta-cyclodextrin stationary phase filler chromatographic column (Coating CP chromatography il Dex CB column), the length of the chromatographic column is 25m, the inner diameter is 0.25mm, and the thickness of the stationary phase membrane is 0.39 mu m; the sample injection amount is 0.1-1.0 mu L; the carrier gas is high-purity helium, and the purity of the carrier gas is more than or equal to 99.999 percent; the flow rate of the carrier gas is 2.0-4.0 mL/min; the sample injection mode is divided sample injection, and the dividing ratio is 50: 1; the temperature of the sample inlet is 250-300 ℃; the detector is a flame ionization detector; the temperature of the detector is 250-300 ℃; the temperature rising procedure is as follows: the initial temperature is 40-70 deg.C, and is maintained for 1-3min, and the temperature is increased to 200 deg.C at a rate of 5-15 deg.C/min, and is maintained for 10-30 min.
The peak area normalization method comprises the following steps: and (3) detecting the finished product sample of the R-glyceraldehyde acetonide by GC-FID, respectively calculating the chromatographic peak areas of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide, and calculating the sum of the areas of the chromatographic peaks in the finished product of the R-glyceraldehyde acetonide to obtain the total chromatographic peak area. Then, the chromatographic peak area of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide is divided by the total chromatographic peak area to obtain the percentage of the chromatographic peak area of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide to the total chromatographic peak area, which is the relative content of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide.
The peak area normalization method is calculated according to a formula (1), wherein the formula (1) is as follows: (Ai/Σ Ai) × 100%, where wi is the relative content of R-glyceraldehyde acetonide or the relative content of S-glyceraldehyde acetonide in the finished R-glyceraldehyde acetonide sample; ai is the chromatographic peak area of R-glyceraldehyde acetonide or the chromatographic peak area of S-glyceraldehyde acetonide in the R-glyceraldehyde acetonide finished product sample; sigma Ai is the total chromatographic peak area in the R-glyceraldehyde acetonide finished product sample.
Example 2
1. Sample pretreatment
And (3) putting the 2.5g R-glyceraldehyde acetonide finished product into a 50mL volumetric flask, adding dichloromethane to dissolve and dilute to a scale mark, and obtaining a liquid to be detected.
2. Preparation of Standard solutions
2.5g of R-glyceraldehyde acetonide standard substance and 2.5g of S-glyceraldehyde acetonide standard substance are respectively taken to be placed in a 50mL volumetric flask, and dichloromethane is added to dissolve and dilute the substances to a scale, so that a standard solution is obtained.
3. Measurement of
And (3) detecting the liquid to be detected prepared in the step (1) and the standard solution prepared in the step (2) by adopting GC-FID, comparing retention time according to the measured value of the standard solution for qualitative determination, determining the R-glyceraldehyde acetonide component and the S-glyceraldehyde acetonide component in the R-glyceraldehyde acetonide finished product, and determining the relative contents of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide in the R-glyceraldehyde acetonide finished product by adopting a peak area normalization method. The specific detection results are shown in FIGS. 1 and 2. As can be seen from FIGS. 1 and 2, the method of the present invention has a very good effect of separating R-glyceraldehyde acetonide from the finished product of R-glyceraldehyde acetonide.
In specific determination, the detection conditions of the GC-FID method are as follows: the chromatographic column is a chemically bonded beta-cyclodextrin stationary phase filler chromatographic column (Coating CP chromatography il Dex CB column), the length of the chromatographic column is 25m, the inner diameter is 0.25mm, and the thickness of the stationary phase membrane is 0.39 mu m; the sample injection amount is 0.2 mu L; the carrier gas is high-purity helium, and the purity of the carrier gas is more than or equal to 99.999 percent; the flow rate of the carrier gas is 3.0 mL/min; the sample injection mode is divided sample injection, and the dividing ratio is 50: 1; the temperature of a sample inlet is 280 ℃; the detector is a flame ionization detector; the temperature of the detector is 300 ℃; the temperature rising procedure is as follows: the initial temperature was 50 ℃ for 2min, and the temperature was raised to 200 ℃ at a rate of 10 ℃/min for 13 min.
The peak area normalization method comprises the following steps: and (3) detecting the finished product sample of the R-glyceraldehyde acetonide by GC-FID, respectively calculating the chromatographic peak areas of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide, and calculating the sum of the areas of the chromatographic peaks in the finished product of the R-glyceraldehyde acetonide to obtain the total chromatographic peak area. Then, the chromatographic peak area of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide is divided by the total chromatographic peak area to obtain the percentage of the chromatographic peak area of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide to the total chromatographic peak area, which is the relative content of R-glyceraldehyde acetonide or S-glyceraldehyde acetonide.
The peak area normalization method is calculated according to a formula (1), wherein the formula (1) is as follows: (Ai/Σ Ai) × 100%, where wi is the relative content of R-glyceraldehyde acetonide or the relative content of S-glyceraldehyde acetonide in the finished R-glyceraldehyde acetonide sample; ai is the chromatographic peak area of R-glyceraldehyde acetonide or the chromatographic peak area of S-glyceraldehyde acetonide in the R-glyceraldehyde acetonide finished product sample; sigma Ai is the total chromatographic peak area in the R-glyceraldehyde acetonide finished product sample.
Example 3
Taking 3 finished product samples of R-glyceraldehyde acetonide produced by different manufacturers, wherein the serial numbers are No. 1, No. 2 and No. 3 respectively, preparing a test sample according to the step 1 in the example 2 and a standard solution according to the step 2, measuring according to the step 3 in the example 2, and calculating the relative percentage contents of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide in the samples respectively through the formula (1). Each sample was tested in parallel 5 times, and the calculation results are shown in tables 1 and 2. As can be seen from tables 1 and 2, the RSD of the method for measuring R-glyceraldehyde acetonide is less than or equal to 0.05 percent, the RSD of the method for measuring S-glyceraldehyde acetonide is less than 0.6 percent, the precision of the measurement result is high, and the reproducibility is good.
Table 1 precision results of measurement of R-glyceraldehyde acetonide (n ═ 5)
TABLE 2 precision results of the measurement of S-glyceraldehyde acetonide (n. 5)
Example 4
Taking a R-glyceraldehyde acetonide standard product, wherein the content of R-glyceraldehyde acetonide is more than or equal to 98.0%, preparing a test sample according to the step 1 in the example 2 and a standard solution according to the step 2, measuring according to the step 3 in the example 2, and calculating the relative percentage content of the R-glyceraldehyde acetonide in the sample according to the formula (1). The parallel measurement is carried out for 5 times, and the calculation results are shown in Table 3. As can be seen from Table 3, the method has the result that the RSD of the R-glyceraldehyde acetonide is less than 0.05 percent and the accuracy of the measurement result is high.
TABLE 3 method accuracy test results confirmation data
Example 5
Taking the finished product sample of R-glyceraldehyde acetonide 1# in example 3, preparing the test sample according to the step 1 and the standard solution according to the step 2 in example 2, respectively adopting isothermal programs set at different temperatures and adopting a peak area normalization method to calculate the relative percentage content of the R-glyceraldehyde acetonide in the sample according to the formula (1) when detecting the test sample by adopting GC-FID, wherein the determination results are shown in Table 4. Meanwhile, the results of the measurement of the finished product sample of R-glyceraldehyde acetonide, No. 1 in example 3, using the temperature rising program are also shown in Table 4.
TABLE 4 measurement results of different set temperature programs
As can be seen from table 4, combining the separation degree of the main peak from the adjacent impurity components, the peak shape, the test time, and the like, the main peak can be effectively separated from the adjacent impurities when the temperature rising process of the preferred conditions is employed in the present invention.
Example 6
The R-glyceraldehyde acetonide standard of example 4 was used as a standard sample, and R-glyceraldehyde acetonide samples numbered 1#, 2#, and 3# of example 3 were measured by the single-point external standard method, and each sample was measured in parallel 5 times under the same chromatographic conditions as example 3, and the measurement results are shown in Table 5.
Table 5 single point external standard sample measurements and precision results (n ═ 5)
Comparing table 5 with table 1, it can be seen that the relative percentage content of R-glyceraldehyde acetonide measured by the single point external standard method in table 5 is similar to that measured by the peak area normalization method in table 1, but the RSD measured by the peak area normalization method in table 1 is significantly better than that measured by the single point external standard method in table 4. Therefore, the quantitative method adopting the peak area normalization method is simple, the result accuracy is high, the precision is high, and the repeatability is good.
In conclusion, the method for detecting the purity of the R-glyceraldehyde acetonide finished product can realize the complete separation of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide, and has the advantages of good precision and accuracy, accurate result, simple quantitative method and good repeatability. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (9)
1. A method for detecting the purity of a finished product of R-glyceraldehyde acetonide comprises the following steps:
1) sample pretreatment: adding an organic solvent into the finished product of the R-glyceraldehyde acetonide for dissolving to obtain a liquid to be detected;
2) preparation of a standard solution: adding an organic solvent into an R-glyceraldehyde acetonide standard substance and an S-glyceraldehyde acetonide standard substance for dissolving to obtain a standard solution;
3) sample detection: respectively detecting the liquid to be detected in the step 1) and the standard solution in the step 2) by adopting a gas chromatography-flame ionization detector method, comparing and retaining time according to the measured value of the standard solution for qualitative determination, determining an R-glyceraldehyde acetonide component and an S-glyceraldehyde acetonide component in the liquid to be detected, and determining the relative contents of the R-glyceraldehyde acetonide and the S-glyceraldehyde acetonide in the liquid to be detected by adopting a peak area normalization method;
in the step 3), a chromatographic column adopted by the GC-FID method is a chemically bonded beta-cyclodextrin stationary phase filler chromatographic column Coating CP chiralsil Dex CB column;
in the step 3), the GC-FID method adopts a temperature rise program comprising: the initial temperature is 40-70 deg.C, and is maintained for 1-3min, and the temperature is increased to 200 deg.C at a rate of 5-15 deg.C/min, and is maintained for 10-30 min.
2. The method for detecting the purity of R-glyceraldehyde acetonide finished product as recited in claim 1, wherein in step 1), the ratio of the mass g of the R-glyceraldehyde acetonide finished product to the volume ml of the organic solvent is 2-3: 50.
3. The method for detecting the purity of the R-glyceraldehyde acetonide finished product according to claim 1, wherein in step 1) or 2), the organic solvent is selected from one of acetone, dichloromethane, ethyl acetate, toluene and acetonitrile.
4. The method for detecting the purity of the R-glyceraldehyde acetonide finished product according to claim 1, wherein in the step 3), the chromatographic column adopted by the GC-FID method is a chemically bonded beta-cyclodextrin stationary phase filler chromatographic column, the length of the chromatographic column is 25m, the inner diameter of the chromatographic column is 0.25mm, and the thickness of the stationary phase membrane is 0.39 μm.
5. The method for detecting the purity of R-glyceraldehyde acetonide finished product according to claim 1, wherein in the step 3), the GC-FID method is performed with a sample amount of 0.1-1.0 μ L; the GC-FID method adopts a split sample injection mode, and the split ratio is 50: 1.
6. The method for detecting the purity of the R-glyceraldehyde acetonide finished product as claimed in claim 1, wherein in the step 3), the carrier gas adopted by the GC-FID method is high-purity helium gas, and the purity of the carrier gas is more than or equal to 99.999%; the carrier gas flow rate adopted by the GC-FID method is 2.0-4.0 mL/min.
7. The method as claimed in claim 1, wherein in step 3), the GC-FID method employs a sample inlet temperature of 250-300 ℃.
8. The method for detecting the purity of R-glyceraldehyde acetonide finished product as claimed in claim 1, wherein the GC-FID method in step 3) employs a detector temperature of 250-300 ℃.
9. The method for detecting the purity of R-glyceraldehyde acetonide finished product according to claim 1, wherein in the step 3), the peak area normalization method is calculated according to formula (1), and the formula (1) is: (Ai/Σ Ai) × 100%, where wi is the relative content of R-glyceraldehyde acetonide or the relative content of S-glyceraldehyde acetonide in the finished R-glyceraldehyde acetonide sample; ai is the chromatographic peak area of R-glyceraldehyde acetonide or the chromatographic peak area of S-glyceraldehyde acetonide in the R-glyceraldehyde acetonide finished product sample; sigma Ai is the total chromatographic peak area in the R-glyceraldehyde acetonide finished product sample.
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