A method for detecting the content of S-2-octanol and its enantiomers by derivatization

Through the gas chromatography-flame ionization detector method (GC-FID) combined with the peak area normalization method, the problem of the inability to accurately detect chiral isomers in the S-2-octanol finished products in the prior art was solved, and the accurate separation and quantitative analysis of S-2-octanol and R-2-octanol were achieved, which improved the accuracy and accuracy of the detection.

CN116223706BActive Publication Date: 2025-04-22SHANGHAI CHEMSPEC CORP
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Patent Information

Application Number
CN202211678794.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-12-26
Publication Date
2025-04-22
Estimated Expiration
2042-12-26

AI Technical Summary

Technical Problem

The existing purity detection methods for S-2-octanol finished products cannot accurately separate chiral isomers, resulting in inaccurate detection results and affecting the quality of downstream products.

Method used

Complete separation and quantitative analysis of S-2-octanol and R-2-octanol were achieved by mixing the S-2-octanol product sample with appropriate solvents and derivatization reagents using gas chromatography-flame ionization detector method (GC-FID) combined with peak area normalization method.

Benefits of technology

Accurate detection of S-2-octanol and R-2-octanol in S-2-octanol finished products is achieved, improving the precision and accuracy of the detection and ensuring the quality of downstream products.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a method for detecting the content of S-2-octanol and its enantiomers by derivatization, comprising: adding a finished S-2-octanol sample to a first solvent, a second solvent and a derivatization reagent to obtain a test solution after mixing, detecting by gas chromatography-flame ionization detector method, and determining the relative content of S-2-octanol and R-2-octanol in the test solution by peak area normalization method. The method for detecting the content of S-2-octanol and its enantiomers by derivatization provided by the present invention can achieve complete separation of S-2-octanol and R-2-octanol, the method has good precision and accuracy, the result is accurate, the quantitative method is simple, and the repeatability is good.
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Description

Technical Field

[0001] The invention belongs to the technical field of purity detection of organic compounds, and relates to a method for detecting the content of S-2-octanol and its enantiomers by derivatization, and specifically to a method for detecting the content of S-2-octanol and R-2-octanol in a finished S-2-octanol product. Background Art

[0002] S-2-octanol, also known as S-(+)-2-nonanol, is called 2-Octanol (S) in English, and its molecular formula is C 8 H 18 O, CAS No. 6169-06-8, is a chemical intermediate that can be widely used in the manufacture of plasticizers, synthetic fiber oils, defoamers, mining flotation agents, pesticide emulsifiers and fragrances. It can also be used as a solvent for grease and wax. It is used as a solvent for nitro spray paint and enamel to improve ductility, gloss and fluidity. It is also used as a fiber wetting agent, brake oil, demulsifier and a raw material for the manufacture of plasticizers and fragrances.

[0003] At present, due to the process of preparing S-2-octanol finished product, a small amount of R-2-octanol will be produced, and the currently existing S-2-octanol finished product purity detection method is gas chromatography, and conventional polarity, medium polarity or non-polar chromatographic columns cannot separate chiral isomers, making the S-2-octanol finished product purity detection result inaccurate. When the S-2-octanol containing R-2-octanol is further prepared into downstream chiral compounds, its isomer is difficult to separate, and finally affects the quality of downstream products. Therefore, setting up a kind of simple and accurate detection method for the mensuration of S-2-octanol and R-2-octanol relative content is of great significance for S-2-octanol quality monitoring. Summary of the invention

[0004] In view of the above-mentioned shortcomings of the prior art, the object of the present invention is to provide a method for detecting the content of S-2-octanol and its enantiomers by derivatization, which can effectively detect the content of S-2-octanol and R-2-octanol in the finished S-2-octanol product, thereby effectively controlling the purity of S-2-octanol in the finished S-2-octanol product.

[0005] To achieve the above-mentioned object and other related objects, the present invention provides a method for detecting the content of S-2-octanol and its enantiomers by derivatization, comprising: adding a finished S-2-octanol sample to a first solvent, a second solvent and a derivatization reagent to obtain a test solution, detecting the solution by gas chromatography-flame ionization detector (GC-FID), and determining the relative contents of S-2-octanol and R-2-octanol in the test solution by peak area normalization.

[0006] Preferably, in the finished S-2-octanol product, the CAS number of the S-2-octanol is 6169-06-8, and the CAS number of the R-2-octanol is 5978-70-1.

[0007] Preferably, the S-2-octanol finished product sample is first added to a first solvent to dissolve and then a second solvent and a derivatization reagent are sequentially added and mixed evenly.

[0008] More preferably, the mixing shaking time is 9-11 minutes, preferably 10 minutes.

[0009] Preferably, the first solvent is selected from at least one of tetrahydrofuran, acetonitrile, toluene or chlorobenzene.

[0010] Preferably, the second solvent is anhydrous pyridine.

[0011] Preferably, the derivatization agent is bis(trimethylsilyl)trifluoroacetamide (BSTFA, CAS No. 25561-30-2).

[0012] Preferably, the volume ratio of the S-2-octanol finished product sample to the first solvent is 1:5-20, specifically 1:5-10, 1:10-15, 1:15-20.

[0013] Preferably, the volume ratio of the S-2-octanol finished product sample to the second solvent added is 1:0.5-2, specifically 1:0.5-1, 1:1-1.5, 1:1.5-2.

[0014] Preferably, the volume ratio of the S-2-octanol finished product sample to the derivatization reagent added is 1:5-15, specifically 1:5-8, 1:8-12, 1:12-15.

[0015] Preferably, the detection is performed using a gas chromatography-flame ionization detector (GC-FID), comprising the following steps:

[0016] 1) Providing a positioning solution: the positioning solution includes an S-2-octanol standard, an R-2-octanol standard, a first solvent, a second solvent and a derivatization reagent;

[0017] 2) Sample detection: The solution to be tested and the positioning solution in step 1) are detected respectively by gas chromatography-flame ionization detector (GC-FID), and the retention time of the positioning solution and the solution to be tested is compared for qualitative analysis, and the peak positions of S-2-octanol and R-2-octanol in the solution to be tested are determined, and then the peak area normalization method is used for quantitative analysis to determine the relative contents of S-2-octanol and R-2-octanol in the solution to be tested.

[0018] More preferably, in step 1), the positioning solution is obtained by first adding the S-2-octanol standard and the R-2-octanol standard into a first solvent to dissolve them, and then sequentially adding a second solvent and a derivatization reagent to mix them evenly.

[0019] Further preferably, the shaking time of the mixing is 9-11 minutes, preferably 10 minutes.

[0020] More preferably, in step 1), the S-2-octanol standard is produced by TCI (Shanghai) Chemical Industry Development Co., Ltd. In the S-2-octanol standard, the content of S-2-octanol is ≥ 99.0 v / v%.

[0021] More preferably, in step 1), the R-2-octanol standard is produced by TCI (Shanghai) Chemical Industry Development Co., Ltd. The R-2-octanol standard also contains S-2-octanol.

[0022] More preferably, in step 1), the first solvent is selected from at least one of tetrahydrofuran, acetonitrile, toluene or chlorobenzene.

[0023] More preferably, in step 1), the second solvent is anhydrous pyridine.

[0024] More preferably, in step 1), the derivatization agent is bis(trimethylsilyl)trifluoroacetamide (BSTFA, CAS No. 25561-30-2).

[0025] More preferably, in step 1), the volume ratio of the S-2-octanol standard to the R-2-octanol standard is 1:0.95-1.05, preferably 1:1.

[0026] More preferably, in step 1), the volume ratio of the S-2-octanol standard to the first solvent is 1:5-20, specifically 1:5-10, 1:10-15, 1:15-20.

[0027] More preferably, in step 1), the volume ratio of the S-2-octanol standard to the second solvent is 1:0.5-2, specifically 1:0.5-1, 1:1-1.5, 1:1.5-2.

[0028] More preferably, in step 1), the volume ratio of the S-2-octanol standard to the derivatization reagent is 1:5-15, specifically 1:5-8, 1:8-12, 1:12-15.

[0029] More preferably, in step 2), in the GC-FID method, the detector is a flame ionization detector (hydrogen flame detector, FID), and the detector temperature is 250-300°C, specifically 250-280°C, 280-300°C, preferably 280°C.

[0030] More preferably, in step 2), in the GC-FID method, the chromatographic column is a CP chirasil Dex CB capillary chromatographic column (20-30m×0.20-0.30mm×0.20-0.30μm, column length×inner diameter×stationary phase film thickness), and the filler is a chemically bonded beta-cyclodextrin stationary phase.

[0031] Further preferably, the chromatographic column is a CP chirasil Dex CB capillary chromatographic column (25m×0.25mm×0.25μm, column length×inner diameter×stationary phase film thickness), and the filler is a chemically bonded beta-cyclodextrin stationary phase.

[0032] More preferably, in step 2), in the GC-FID method, the temperature program used is: the initial temperature is 70-90°C and maintained for 0-2min, then the temperature is increased to 95-100°C at a rate of 1-2°C / min, maintained for 0-5min, and then the temperature is increased to 180-200°C at a rate of 15-25°C / min, and maintained for 0-10min.

[0033] More preferably, in step 2), the GC-FID method further comprises the following detection conditions:

[0034] The injection port temperature is 250-300°C, preferably 250°C; the injection volume is 0.1-1.0μL, preferably 0.2μL; the carrier gas is high-purity nitrogen, and the carrier gas purity is ≥99.999%; the carrier gas flow rate is 1.0-2.0mL / min, preferably 1.0mL / min; the injection method is split injection, and the split ratio is 50-100:1, preferably 80:1.

[0035] Preferably, the peak area normalization method refers to: after the solution to be tested is detected by GC-FID, the chromatographic peak areas of S-2-octanol and R-2-octanol in the solution to be tested are calculated respectively, and the sum of the two chromatographic peak areas is calculated to obtain the total chromatographic peak area. Then, the chromatographic peak area of ​​S-2-octanol or R-2-octanol is divided by the total chromatographic peak area, respectively, to obtain the percentage of the chromatographic peak area of ​​S-2-octanol or R-2-octanol to the total chromatographic peak area, which is the relative content of benzene S-2-octanol or R-2-octanol in the solution to be tested.

[0036] Preferably, the peak area normalization method is calculated according to formula (1):

[0037] The formula (1) is:

[0038] In the formula, w i A is the relative content of S-2-octanol or the relative content of R-2-octanol in the test solution; i is the chromatographic peak area of ​​S-2-octanol or the chromatographic peak area of ​​R-2-octanol in the test solution; ∑A i It is the sum of the chromatographic peak areas of S-2-octanol and R-2-octanol in the test solution.

[0039] As described above, the present invention provides a method for detecting the content of S-2-octanol and its enantiomers by derivatization, using gas chromatography-flame ionization detector (GC-FID) to detect S-2-octanol and R-2-octanol in the finished S-2-octanol product, and through the preferred detection conditions, it is possible to achieve complete separation of S-2-octanol and R-2-octanol as chiral isomers, making up for the shortcomings of the current detection method of the product, the method has good precision and accuracy, and the result is accurate. The detection method adopts the peak area normalization method for quantification, and the quantitative method is simple and has good repeatability. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 The gas chromatogram shown is a gas chromatogram of the determination of S-2-octanol and R-2-octanol in the S-2-octanol finished product by the method of the present invention, wherein a is R-2-octanol and b is S-2-octanol.

[0041] Figure 2 It shows the gas chromatogram of the determination of S-2-octanol and R-2-octanol in the R-2-octanol standard by the method of the present invention, wherein a is R-2-octanol and b is S-2-octanol.

[0042] Figure 3 Shown is a gas chromatogram of a finished sample of S-2-octanol without derivatization.

[0043] Figure 4 Shown is a gas chromatogram of a derivatized S-2-octanol product sample using gas chromatography conditions not in the present invention. DETAILED DESCRIPTION

[0044] The present invention is further described below in conjunction with specific examples. It should be understood that these examples are only used to illustrate the present invention and are not used to limit the scope of protection of the present invention.

[0045] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.

[0046] The reagents and instruments used in the following examples are as follows:

[0047] 1. Reagents

[0048] Finished S-2-octanol (commercially available); S-2-octanol standard (S-2-octanol content ≥ 99.0 v / v%, TCI (Shanghai) Chemical Industry Development Co., Ltd.); R-2-octanol standard (containing S-2-octanol, TCI (Shanghai) Chemical Industry Development Co., Ltd.); tetrahydrofuran, acetonitrile, toluene, chlorobenzene (chromatographically pure, Shanghai Anpu Laboratory Technology Co., Ltd.); anhydrous pyridine (chromatographically pure, Merck); BSTFA (chromatographically pure, Merck).

[0049] 2. Instruments

[0050] Agilent 7890A gas chromatograph (Agilent, USA) equipped with a flame ionization detector; Agilent CP chirasil Dex CB capillary column (25m×0.25mm, 0.25μm, filled with chemically bonded beta-cyclodextrin stationary phase) (Agilent, USA).

[0051] Example 1

[0052] 1. Sample pretreatment

[0053] Take 0.5 mL of S-2-octanol finished product sample, add 5 mL of acetonitrile to dissolve, then add 0.5 mL of anhydrous pyridine and 5 mL of BSTFA in sequence, mix well, and shake for 10 minutes to obtain the test solution 1.

[0054] 2. Preparation of positioning solution

[0055] Take 0.5 mL of S-2-octanol standard and 0.5 mL of R-2-octanol standard respectively, add 5 mL of acetonitrile to dissolve, then add 0.5 mL of anhydrous pyridine and 5 mL of BSTFA in sequence, mix well, and shake for 10 minutes to obtain the positioning solution 1*.

[0056] 3. Determination

[0057] Gas chromatography-flame ionization detector (GC-FID) was used to detect the test solution 1 and the positioning solution 1*, and the retention time of the positioning solution 1* and the test solution 1 was compared for qualitative analysis, and the peak positions of S-2-octanol and R-2-octanol in the test solution 1 were determined. Then, the peak area normalization method was used for quantitative analysis to determine the relative contents of S-2-octanol and R-2-octanol in the test solution 1. The specific test results are shown in Figure 1 , 2 .Depend on Figure 1 , 2 It can be seen that the method of the present invention has a good separation effect on S-2-octanol and R-2-octanol in the finished S-2-octanol product.

[0058] Among them, in the GC-FID method, the detector is a flame ionization detector (hydrogen flame detector, FID), and the detector temperature is 280°C. The chromatographic column is a CP chirasil Dex CB capillary column (25m×0.25mm×0.25μm, column length×inner diameter×stationary phase film thickness), and the filler is a chemically bonded beta-cyclodextrin stationary phase. The temperature program used is: the initial temperature is 80°C and maintained for 0min, then the temperature is increased to 95°C at a rate of 1°C / min, maintained for 0min, and then the temperature is increased to 180°C at a rate of 20°C / min, and maintained for 5.75min.

[0059] The GC-FID method also includes the following detection conditions: the injection port temperature is 250°C; the injection volume is 0.2μL; the carrier gas is high-purity nitrogen, and the carrier gas purity is ≥99.999%; the carrier gas flow rate is 1.0mL / min; the injection method is split injection, and the split ratio is 80:1.

[0060] In addition, the peak area normalization method refers to: after the solution 1 to be tested is detected by GC-FID, the chromatographic peak areas of S-2-octanol and R-2-octanol in the solution 1 to be tested are calculated respectively, and the sum of the two chromatographic peak areas is calculated to obtain the total chromatographic peak area. Then, the chromatographic peak area of ​​S-2-octanol or R-2-octanol is divided by the total chromatographic peak area, respectively, to obtain the percentage of the chromatographic peak area of ​​S-2-octanol or R-2-octanol to the total chromatographic peak area, which is the relative content of S-2-octanol or R-2-octanol in the solution 1 to be tested.

[0061] The peak area normalization method is calculated according to formula (1):

[0062] The formula (1) is:

[0063] In the formula, w i A is the relative content of S-2-octanol or the relative content of R-2-octanol in the test solution 1; iis the chromatographic peak area of ​​S-2-octanol or the chromatographic peak area of ​​R-2-octanol in the test solution 1; ∑A i It is the sum of the chromatographic peak areas of S-2-octanol and R-2-octanol in the test solution 1.

[0064] Example 2

[0065] 1. Sample pretreatment

[0066] Take 0.5 mL of S-2-octanol finished product sample, add 2.5 mL of tetrahydrofuran to dissolve, then add 0.25 mL of anhydrous pyridine and 2.5 mL of BSTFA in sequence, mix well, and shake for 9 minutes to obtain the test solution 2.

[0067] 2. Preparation of positioning solution

[0068] Take 0.5 mL of S-2-octanol standard and 0.5 mL of R-2-octanol standard respectively, add 2.5 mL of tetrahydrofuran to dissolve, then add 0.25 mL of anhydrous pyridine and 2.5 mL of BSTFA in sequence, mix well, and shake for 9 minutes to obtain positioning solution 2*.

[0069] 4. Determination

[0070] Gas chromatography-flame ionization detector (GC-FID) was used to detect the test solution 2 and the positioning solution 2*, respectively. The retention time of the positioning solution 2* and the test solution 2 was compared for qualitative analysis, and the peak positions of S-2-octanol and R-2-octanol in the test solution 2 were determined. Then, the peak area normalization method was used for quantitative analysis to determine the relative contents of S-2-octanol and R-2-octanol in the test solution 2.

[0071] Among them, in the GC-FID method, the detector is a flame ionization detector (hydrogen flame detector, FID), and the detector temperature is 250°C. The chromatographic column is a CP chirasil Dex CB capillary column (25m×0.25mm×0.25μm, column length×inner diameter×stationary phase film thickness), and the filler is a chemically bonded beta-cyclodextrin stationary phase. The temperature program used is: the initial temperature is 70°C and maintained for 1min, then the temperature is increased to 100°C at a rate of 2°C / min, maintained for 5min, and then the temperature is increased to 200°C at a rate of 15°C / min, and maintained for 0min.

[0072] The GC-FID method also includes the following detection conditions: the injection port temperature is 300°C; the injection volume is 0.1μL; the carrier gas is high-purity nitrogen, and the carrier gas purity is ≥99.999%; the carrier gas flow rate is 2.0mL / min; the injection method is split injection, and the split ratio is 50:1.

[0073] In addition, the concept of peak area normalization method and its calculation formula are the same as those in Example 1.

[0074] Example 3

[0075] 1. Sample pretreatment

[0076] Take 0.5 mL of S-2-octanol finished product sample, add 10 mL of toluene to dissolve it, then add 1 mL of anhydrous pyridine and 7.5 mL of BSTFA in sequence, mix well, and shake for 11 minutes to obtain the test solution 3.

[0077] 2. Preparation of positioning solution

[0078] Take 0.5 mL of S-2-octanol standard and 0.5 mL of R-2-octanol standard respectively, add 10 mL of toluene to dissolve, then add 1 mL of anhydrous pyridine and 7.5 mL of BSTFA in sequence, mix well, and shake for 11 minutes to obtain the positioning solution 3*.

[0079] 5. Determination

[0080] Gas chromatography-flame ionization detector (GC-FID) was used to detect the test solution 3 and the positioning solution 3*, respectively. The retention time of the positioning solution 3* and the test solution 3 was compared for qualitative analysis, and the peak positions of S-2-octanol and R-2-octanol in the test solution 3 were determined. Then, the peak area normalization method was used for quantitative analysis to determine the relative contents of S-2-octanol and R-2-octanol in the test solution 3.

[0081] Among them, in the GC-FID method, the detector is a flame ionization detector (hydrogen flame detector, FID), and the detector temperature is 300°C. The chromatographic column is a CP chirasil Dex CB capillary column (25m×0.25mm×0.25μm, column length×inner diameter×stationary phase film thickness), and the filler is a chemically bonded beta-cyclodextrin stationary phase. The temperature program used is: the initial temperature is 90°C and maintained for 2 minutes, then the temperature is increased to 98°C at a rate of 1.5°C / min, maintained for 3 minutes, and then the temperature is increased to 190°C at a rate of 25°C / min, and maintained for 10 minutes.

[0082] The GC-FID method also includes the following detection conditions: the injection port temperature is 280°C; the injection volume is 1.0 μL; the carrier gas is high-purity nitrogen, and the carrier gas purity is ≥99.999%; the carrier gas flow rate is 1.5 mL / min; the injection method is split injection, and the split ratio is 100:1.

[0083] In addition, the concept of peak area normalization method and its calculation formula are the same as those in Example 1.

[0084] Example 4

[0085] Take three kinds of S-2-octanol finished product samples produced by different manufacturers, numbered 1#, 2#, and 3#, prepare the test solution according to step 1 in Example 1, prepare the positioning solution according to step 2 in Example 1, and measure according to step 3 in Example 1, and calculate the relative percentage content of S-2-octanol and R-2-octanol in the samples by formula (1). Each sample is measured 5 times in parallel, and the calculation results are shown in Tables 1 and 2. As can be seen from Tables 1 and 2, the results of the determination of S-2-octanol by this method have an RSD of less than 0.05%, and the results of the determination of R-2-octanol have an RSD of less than 2%, and the determination results have high precision and good reproducibility.

[0086] Table 1 Precision results of S-2-octanol determination of samples (n=5)

[0087]

[0088] Table 2 Precision results of sample determination of R-2-octanol (n=5)

[0089]

[0090] Example 5

[0091] Take S-2-octanol standard, wherein the content of S-2-octanol is ≥99.0%, prepare the test solution according to step 1 in Example 1, prepare the positioning solution according to step 2 in Example 1, and perform the determination according to step 3 in Example 1, and calculate the relative percentage content of S-2-octanol in the sample by formula (1). Parallel determination is performed 5 times, and the calculation results are shown in Table 3. As can be seen from Table 3, the result of determining S-2-octanol by this method has an RSD of <0.01%, and the determination result has high accuracy.

[0092] Table 3 Method accuracy test results confirmation data

[0093]

[0094] Example 6

[0095] Take the S-2-octanol finished product sample numbered 1# in Example 4, prepare the test solution according to step 1 in Example 1, prepare the positioning solution according to step 2 in Example 1, and then use GC-FID to detect the test sample, respectively use isothermal programs with different temperature settings, and use the peak area normalization method to calculate the relative percentage content of S-2-octanol in the sample according to formula (1), and the measurement results are shown in Table 4. At the same time, the measurement results of the S-2-octanol finished product sample numbered 1# in Example 4 using the temperature program are also listed in Table 4.

[0096] Table 4 Test results of different set temperature programs

[0097]

[0098] It can be seen from Table 4 that, considering the separation degree between the main peak and the adjacent impurity components and the test time and other factors, when the temperature rise program of the preferred conditions is adopted in the present invention, the main peak and the target impurity can be effectively separated.

[0099] Example 5

[0100] Take the S-2-octanol finished product sample numbered 1# in Example 4, prepare the test solution according to step 1 in Example 1 without adding the derivatization reagent, prepare the positioning solution according to step 2 in Example 1, and perform the measurement according to step 3 in Example 1. The measurement results are shown in Figure 3 .Depend on Figure 3 It can be seen that after the measurement by the above method, S-2-octanol and R-2-octanol cannot be separated.

[0101] Take the S-2-octanol finished product sample numbered 1# in Example 4, prepare the test solution according to step 1 in Example 1, prepare the positioning solution according to step 2 in Example 1, and then perform the measurement according to step 3 in Example 1. In the specific measurement, the gas chromatography conditions such as the chromatographic column in the present invention are not selected, and the measurement results are shown in Figure 4 .Depend on Figure 4 It can be seen that after the measurement by the above method, S-2-octanol and R-2-octanol cannot be separated.

[0102] In summary, the method for detecting the content of S-2-octanol and its enantiomers by derivatization provided by the present invention can achieve complete separation of S-2-octanol and R-2-octanol, and the method has good precision and accuracy, accurate results, simple quantitative method and good repeatability. Therefore, the present invention effectively overcomes various shortcomings in the prior art and has high industrial utilization value.

[0103] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.

Claims

1. A method for detecting the content of S-2-octanol and its enantiomers by derivatization, comprising: The S-2-octanol finished product sample is added to the first solvent, the second solvent and the derivatization reagent to obtain a test solution, and the GC-FID method is used for detection, and the relative contents of S-2-octanol and R-2-octanol in the test solution are determined by the peak area normalization method; The S-2-octanol finished product sample is first added to the first solvent to dissolve, and then the second solvent and the derivatization reagent are added in sequence and mixed evenly; The first solvent is selected from at least one of tetrahydrofuran, acetonitrile, toluene or chlorobenzene; the second solvent is anhydrous pyridine; the derivatization agent is bis(trimethylsilyl)trifluoroacetamide; In the GC-FID method, the chromatographic column is a CP chirasil Dex CB capillary chromatographic column, 20-30m×0.20-0.30mm×0.20-0.30µm, column length×inner diameter×stationary phase film thickness, and the filler is a chemically bonded beta-cyclodextrin stationary phase; In the GC-FID method, the temperature program used is: the initial temperature is 70-90°C and maintained for 0-2 min, then the temperature is increased to 95-100°C at a rate of 1-2°C / min, maintained for 0-5 min, and then the temperature is increased to 180-200°C at a rate of 15-25°C / min, and maintained for 0-10 min.

2. The method for detecting the content of S-2-octanol and its enantiomers by derivatization according to claim 1, characterized in that: Includes any one or more of the following conditions: A1) The shaking time of the mixing is 9-11 minutes; A2) the volume ratio of the S-2-octanol finished product sample to the first solvent added is 1:5-20; A3) the volume ratio of the S-2-octanol finished product sample to the second solvent added is 1:0.5-2; A4) The volume ratio of the S-2-octanol finished sample to the derivatization reagent is 1:5-15.

3. The method for detecting the content of S-2-octanol and its enantiomers by derivatization according to claim 1, characterized in that: The detection was carried out by gas chromatography-flame ionization detector method, including the following steps: 1) Providing a positioning solution: the positioning solution includes an S-2-octanol standard, an R-2-octanol standard, a first solvent, a second solvent and a derivatization reagent; 2) Sample detection: Use GC-FID method to detect the solution to be tested and the positioning solution in step 1) respectively, compare the retention time of the positioning solution and the solution to be tested for qualitative analysis, determine the peak positions of S-2-octanol and R-2-octanol in the solution to be tested, and then use the peak area normalization method for quantitative analysis to determine the relative contents of S-2-octanol and R-2-octanol in the solution to be tested.

4. The method for detecting the content of S-2-octanol and its enantiomers by derivatization according to claim 3, characterized in that: Step 1) includes any one or more of the following conditions: B1) The positioning solution is obtained by first adding the S-2-octanol standard and the R-2-octanol standard to a first solvent for dissolution and then sequentially adding a second solvent and a derivatization reagent and mixing them evenly; B2) the first solvent is selected from at least one of tetrahydrofuran, acetonitrile, toluene or chlorobenzene; B3) the second solvent is anhydrous pyridine; B4) the derivatization reagent is bis(trimethylsilyl)trifluoroacetamide; B5) the volume ratio of the S-2-octanol standard to the R-2-octanol standard is 1:0.95-1.05; B6) the volume ratio of the S-2-octanol standard to the first solvent is 1:5-20; B7) the volume ratio of the S-2-octanol standard to the second solvent added is 1:0.5-2; B8) The volume ratio of the S-2-octanol standard to the derivatization reagent is 1:5-15.

5. The method for detecting the content of S-2-octanol and its enantiomers by derivatization according to claim 3, characterized in that: In step 2), in the GC-FID method, the detector is a flame ionization detector, and the detector temperature is 250-300°C.

6. The method for detecting the content of S-2-octanol and its enantiomers by derivatization according to claim 3, characterized in that: The GC-FID method also includes the following detection conditions: the injection port temperature is 250-300°C; the injection volume is 0.1-1.0µL; the carrier gas is high-purity nitrogen, and the carrier gas purity is ≥99.999%; the carrier gas flow rate is 1.0-2.0mL / min; the injection method is split injection, and the split ratio is 50-100:

1.

7. The method for detecting the content of S-2-octanol and its enantiomers by derivatization according to claim 1, characterized in that: The peak area normalization method is calculated according to formula (1): The formula (1) is: , In the formula, w i is the relative content of S-2-octanol or the relative content of R-2-octanol in the solution to be tested; A i is the chromatographic peak area of ​​S-2-octanol or the chromatographic peak area of ​​R-2-octanol in the test solution; It is the sum of the chromatographic peak areas of S-2-octanol and R-2-octanol in the test solution.

Citation Information

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