Method for simultaneously detecting purity and impurities of 3-chloro-1-propanol

Abstract

The invention discloses a method for simultaneously detecting the purity and impurities of 3-chloro-1-propanol, and relates to the technical field of chemical analysis, the method comprises the following steps: the impurities comprise 1, 3-dichloropropane, 1, 7-dichloro-4-oxaheptane and 3-(3-chloropropoxy) propan-1-ol, and the method comprises the following steps: S1, preparing a test solution; s2, preparing a reference substance solution; s3, gas chromatography determination: respectively carrying out gas chromatography detection on the reference substance solution prepared in the step S2 and the test solution prepared in the step S1, and recording chromatograms; s4, calculating the contents of 1, 3-dichloropropane, 1, 7-dichloro-4-oxaheptane and 3-(3-chloropropoxy) propyl-1-alcohol in the test sample by adopting an external standard method according to the peak area and concentration of each substance in the reference substance solution and the peak area of the corresponding substance in the test sample solution; the purity of the 3-chloro-1-propanol is calculated by adopting an area normalization method, so that the problem that the purity and impurities of the 3-chloro-1-propanol cannot be detected at the same time in the prior art is solved.

Description

Technical Field

[0001] This invention relates to the field of chemical analysis technology, specifically to a method for simultaneously detecting the purity of 3-chloro-1-propanol and its impurities. Background Technology

[0002] In the field of modern drug synthesis, the quality of starting materials directly determines the success or failure of subsequent drug research and production. 3-Chloro-1-propanol, as an important starting material for drug synthesis, plays an indispensable role in the preparation of many clinical drugs due to its unique chemical structure and reactivity. This compound can participate in the construction of drug molecules as a key intermediate. For example, in the synthesis of the expectorant fodostatin, the participation of 3-chloro-1-propanol provides the necessary chemical basis for the formation of the drug's active structure, and its quality stability is directly related to the continuity and controllability of drug production.

[0003] For starting materials used in drug synthesis, purity is a core indicator of quality, and the purity level of 3-chloro-1-propanol directly affects the structural integrity and pharmacological activity of the final product. In drug synthesis reaction systems, trace impurities in 3-chloro-1-propanol can trigger a series of quality risks by participating in side reactions and interfering with reaction equilibrium: First, impurities may cause stereoconfiguration deviations in drug molecules, and stereoisomers often have different pharmacological effects, and may even be toxic; second, the presence of impurities can reduce the purity of the target drug, leading to abnormal absorption and distribution in the body, resulting in decreased bioavailability and affecting therapeutic efficacy; more seriously, some impurities may act as exogenous foreign bodies, triggering an immune response in the body, posing potential immunogenic risks and threatening drug safety. Therefore, establishing strict quality control standards for 3-chloro-1-propanol, especially developing highly sensitive and selective impurity detection methods, has become a crucial link in ensuring the quality of the active pharmaceutical ingredient and the safety of clinical use.

[0004] However, there is no publicly available method for simultaneous detection of the purity and impurities of 3-chloro-1-propanol. Existing detection technologies mostly focus on the determination of a single indicator or can only perform qualitative or quantitative analysis on a few known impurities, which cannot meet the multi-dimensional and comprehensive quality control requirements of starting materials in the drug synthesis process.

[0005] Based on the above situation, we will develop a method that can simultaneously determine the purity of 3-chloro-1-propanol and accurately detect impurities, filling the gap in existing technology. This method is of great practical significance and application value for improving the quality control system of 3-chloro-1-propanol and ensuring the production quality and medication safety of downstream drugs. Summary of the Invention

[0006] The purpose of this invention is to solve the problem that the purity and impurities of 3-chloro-1-propanol cannot be detected simultaneously in the prior art. This invention proposes a method for simultaneously detecting the purity and impurities of 3-chloro-1-propanol. This method can quantitatively detect the purity and impurities of 3-chloro-1-propanol, and the analytical results are reliable.

[0007] This invention is achieved through the following technical solution: A method for simultaneously determining the purity of 3-chloro-1-propanol and its impurities, wherein the impurities include 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane, and 3-(3-chloropropoxy)prop-1-ol, the method comprising the following steps: S1. Preparation of test solution: Accurately weigh an appropriate amount of 3-chloro-1-propanol test sample, dissolve and dilute it with anhydrous ethanol to obtain the test solution; S2. Preparation of reference solution: Accurately weigh appropriate amounts of 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane and 3-(3-chloropropoxy)prop-1-ol reference standards, dissolve and dilute with anhydrous ethanol to obtain a mixed reference solution containing the three impurities. S3. Gas chromatography determination: The reference solution prepared in step S2 and the test solution prepared in step S1 are respectively subjected to gas chromatography detection and the chromatograms are recorded. In gas chromatography separation, the resolution between 3-chloro-1-propanol and each impurity substance is ≥1.5. S4. Result Calculation: Based on the peak area and concentration of each substance in the reference solution and the peak area of ​​the corresponding substance in the test solution, the contents of 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane and 3-(3-chloropropoxy)prop-1-ol in the test sample are calculated using the external standard method; at the same time, the purity of 3-chloro-1-propanol is calculated using the area normalization method.

[0008] Furthermore, in step S1, the sample weight of 3-chloro-1-propanol is 0.1~1g, and the dissolution volume of anhydrous ethanol is 5~50mL.

[0009] Furthermore, in step S2, the concentrations of 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane, and 3-(3-chloropropoxy)prop-1-ol in the mixed reference solution are all 10~30 μg / mL.

[0010] Furthermore, in step S3, the detector temperature for gas chromatography detection is 200~300℃; the gas chromatography detection uses an FID flame ionization detector and a polar capillary column.

[0011] Furthermore, in step S3, the injection port temperature for gas chromatography detection is 100~200℃, the carrier gas flow rate is 1.0~2.0mL / min, the split ratio is 5~15:1, and the injection volume is 1~8μL.

[0012] Furthermore, in step S3, the gas chromatographic detection uses the following temperature conditions: The initial temperature of the chromatographic column was 120℃, and maintained for 2 min. Increase the temperature to 150°C at a rate of 10°C per minute and maintain the temperature for 1 minute; The temperature was increased to 154°C at a rate of 1°C per minute, and then increased to 162°C at a rate of 0.5°C per minute. Finally, the temperature is increased to 252°C at a rate of 20°C per minute and maintained for 2 minutes.

[0013] Furthermore, in step S3, gas chromatography detection is performed using gradient elution.

[0014] Furthermore, the solvents used in preparing the reference solution and the test solution were both anhydrous ethanol, and the solvent specifications were consistent.

[0015] Furthermore, in step S4, when calculating the purity of 3-chloro-1-propanol, the formula for the area normalization method is: Purity of 3-chloro-1-propanol = (Peak area of ​​3-chloro-1-propanol / Sum of the areas of all peaks) × 100%; The formula for calculating the impurity of 3-chloro-1-propanol is as follows: 3-Chloro-1-propanol impurity content = (A) 供试品 ×C 对照品 ) / ( A 对照品 ×C 供试品 ) ×100%, Among them, A 供试品 Represents the peak area of ​​the test sample; C 对照品 Represents the concentration of the reference standard; A 对照品 Represents the area of ​​the control peak; C 供试品 This represents the concentration of the test sample 3-chloro-1-propanol.

[0016] Compared with the prior art, the present invention has the following advantages and beneficial effects: I. This invention proposes a method for simultaneously detecting the purity of 3-chloro-1-propanol and its impurities, which can achieve accurate determination of the purity of the main component of 3-chloro-1-propanol, and simultaneously quantitatively detect the content of its key related substances 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane and 3-(3-chloropropoxy)prop-1-ol. Compared to existing technologies, this method offers several advantages: First, it fills the gap in current technologies that struggle to simultaneously detect both the purity of the main component of 3-chloro-1-propanol and the content of target impurities. It eliminates the need for multiple batch tests, enabling a comprehensive characterization of both the main component and key impurities in a single step, significantly improving detection efficiency and reducing costs and operational complexity. Second, it combines high sensitivity and high selectivity, effectively avoiding interference between impurities and between impurities and the main component. It achieves precise quantification even for low-content impurities, and the accuracy, repeatability, and stability of the detection data meet the stringent requirements of API quality control, providing a scientific and reliable analytical basis for product quality assessment. Third, it focuses on the core needs of API quality research and production process control. Through comprehensive monitoring of the purity of the main component of 3-chloro-1-propanol and key impurities, it effectively ensures the safety and quality uniformity of APIs, providing crucial technical support for the quality control systems of pharmaceutical manufacturers. This has significant practical implications for raw material quality research and industrial applications in the pharmaceutical and chemical industries.

[0017] Second, this invention proposes a method for simultaneously detecting the purity of 3-chloro-1-propanol and its impurities, which breaks through the limitations of existing technologies that mostly use single detection or step-by-step detection. It integrates the determination of the main purity and the quantification of three characteristic impurities into a single detection system, eliminating the need to split the detection process, greatly improving detection efficiency, reducing detection costs and operational complexity, and meeting the actual needs of "one-stop" detection in the quality control of active pharmaceutical ingredients.

[0018] Third, this invention proposes a method for simultaneously detecting the purity of 3-chloro-1-propanol and its impurities. By optimizing the detection conditions (such as chromatographic separation parameters), the method ensures excellent separation between the main component and each impurity, effectively avoids interference between components, and the detection results have high accuracy, high precision and good repeatability. At the same time, the method has high sensitivity and high selectivity, and can accurately capture trace impurities, providing reliable data support for the effective control of impurities.

[0019] Fourth, this invention proposes a method for simultaneously detecting the purity of 3-chloro-1-propanol and its impurities. Establishing a highly sensitive and selective impurity detection method is a core link in the quality control of active pharmaceutical ingredients (APIs). This method specifically addresses the technical requirement for simultaneous control of the main purity and key impurities in the quality research of 3-chloro-1-propanol APIs, effectively ensuring the quality stability and safety of APIs and laying the foundation for the quality controllability of subsequent formulations. It has significant practical value and broad application prospects in the fields of raw material quality testing, process optimization, and compliance control in the pharmaceutical and chemical industries. Attached Figure Description

[0020] Figure 1 This is the chromatogram of the blank reagent.

[0021] Figure 2 This is the chromatogram of the reference solution.

[0022] Figure 3 This is the chromatogram of the test solution.

[0023] Figure 4 It is a specific location map. Detailed Implementation

[0024] The present invention will be further described in detail below with reference to embodiments, but the implementation of the present invention is not limited thereto.

[0025] Example 1 To facilitate public understanding of the present invention, this embodiment uses a method for simultaneously detecting the purity of 3-chloro-1-propanol and its impurities as an example to further illustrate the present solution.

[0026] In this embodiment, the purity of 3-chloro-1-propanol and its impurities were determined by the following steps: Step 1: Preparation of the test solution: Accurately weigh 500 mg of the test sample, place it in a 25 mL volumetric flask, dissolve it in anhydrous ethanol, and quantitatively dilute it to approximately 20 mg of 3-chloro-1-propanol per 1 mL.

[0027] Blank solution: anhydrous ethanol.

[0028] Step 2: Preparation of the reference solution: Accurately weigh appropriate amounts of 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane, and 3-(3-chloropropoxy)prop-1-ol reference standards, dissolve them in anhydrous ethanol, and quantitatively dilute them to a solution containing approximately 20 μg each of the impurities 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane, and 3-(3-chloropropoxy)prop-1-ol per mL.

[0029] Step 3: Gas chromatography determination.

[0030] The blank solution, reference solution, and test solution were analyzed under the following chromatographic conditions, and the chromatograms were recorded (e.g., ...). Figures 1-3 (As shown).

[0031] The chromatographic conditions are as follows: The gas phase was Thermo Fisher Scientific TRACE 1600; The chromatographic column used was SH-PolarD, 30m × 0.32mm × 0.5μm; The solvent is anhydrous ethanol; The detector is an FID (flame ionization detector). The detector temperature is 250℃; The injection port temperature is 200℃; The carrier gas and its flow rate were nitrogen, 1.5 ml / min; The split ratio is 10:1; The injection volume was 4 μL.

[0032] The heating program is as follows: initial temperature 120℃, hold for 2 minutes, increase to 150℃ at a rate of 10℃ per minute, hold for 1 minute; increase to 154℃ at a rate of 1℃ per minute, then increase to 162℃ at a rate of 0.5℃, and finally increase to 252℃ at a rate of 20℃, hold for 2 minutes.

[0033] Step 4: Based on the concentration and peak area of ​​the reference solution and the peak area of ​​the test sample, calculate the content of related substances in the test sample using the external standard method; and determine the purity of 3-chloro-1-propanol using the area normalization method.

[0034] The formula for calculating the purity of 3-chloro-1-propanol using the area normalization method is as follows: Purity of 3-chloro-1-propanol = (Peak area of ​​3-chloro-1-propanol / Sum of all peak areas) × 100%; The formula for calculating the impurity of 3-chloro-1-propanol is as follows: 3-Chloro-1-propanol impurity content = (A) 供试品 ×C 对照品 ) / ( A 对照品 ×C 供试品 ) ×100%, Among them, A 供试品 Represents the peak area of ​​the test sample; C 对照品 Represents the concentration of the reference standard; A 对照品 Represents the area of ​​the control peak; C 供试品 This represents the concentration of the test sample 3-chloro-1-propanol.

[0035] From the above, we can see that the concentration of the 1,3-dichloropropane reference solution is 19.97 μg / mL and its peak area is 0.2731, while the peak area of ​​the test sample is 0.2415. Using the external standard method, the content of 1,3-dichloropropane in the test sample is calculated to be 0.086%. The concentration of the 1,7-dichloro-4-oxaheptane reference solution was 21.34 μg / mL, and the peak area was 0.2484. The peak area of ​​the test sample was 0.0649. The content of 1,7-dichloro-4-oxaheptane in the test sample was calculated to be 0.027% by the external standard method. The concentration of the 3-(3-chloropropoxy)prop-1-ol reference solution was 21.78 μg / mL, and the peak area was 0.2583. The peak area of ​​the test sample was 0.3935. The content of 3-(3-chloropropoxy)prop-1-ol in the test sample was calculated to be 0.159% by the external standard method. The peak area of ​​3-chloro-1-propanol was 245.3553, and the total peak area was 246.055. The purity of 3-chloro-1-propanol was determined to be 99.72% by the area normalization method.

[0036] Methodological validation.

[0037] Methodological validation was conducted in accordance with the analytical method validation guidelines in Appendix (9101) of the 2025 edition of the Chinese Pharmacopoeia and the ICH analytical method validation guidelines. The process and results are as follows: (1) Solution preparation.

[0038] Blank solvent: anhydrous ethanol; Reference solution: Accurately weigh appropriate amounts of 3-chloro-1-propanol, 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane, and 3-(3-chloropropoxy)prop-1-ol reference standards, dissolve them in anhydrous ethanol, and quantitatively dilute to a solution containing approximately 20 mg of 3-chloro-1-propanol and 20 μg each of the impurities 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane, and 3-(3-chloropropoxy)prop-1-ol per mL; Test solution: Accurately weigh 500 mg of the test sample, place it in a 25 mL volumetric flask, dissolve it in anhydrous ethanol and quantitatively dilute it to contain approximately 20 mg of 3-chloro-1-propanol per 1 mL; 1,3-Dichloropropane positioning solution: Accurately weigh 1,3-dichloropropane reference standard, dissolve it in anhydrous ethanol and quantitatively dilute it to approximately 20 μg of 1,3-dichloropropane per 1 mL; 1,7-Dichloro-4-oxaheptane positioning solution: Accurately weigh 1,7-dichloro-4-oxaheptane reference standard, dissolve it in anhydrous ethanol and quantitatively dilute it to contain approximately 20 μg of 1,3-dichloropropane per 1 mL; 3-(3-chloropropoxy)prop-1-ol positioning solution: Accurately weigh 3-(3-chloropropoxy)prop-1-ol reference standard, dissolve it in anhydrous ethanol and quantitatively dilute it to contain about 20 μg of 1,3-dichloropropane per 1 mL; 3-Chloro-1-propanol positioning solution: Accurately weigh 3-chloro-1-propanol reference standard, dissolve it in anhydrous ethanol and quantitatively dilute it to contain approximately 20 μg of 1,3-dichloropropane per 1 mL; (2) The determination conditions for high performance gas chromatography are as follows: The chromatographic column was SH-PolarD, 30m × 0.32mm × 0.5μm; Detector: FID (Flame Ionization Detector); Detector temperature: 250℃; Inlet temperature: 200℃; Flow rate: 1.5 ml / min; Flow split ratio: 10:1; Injection volume: 4 μL; Direct injection, with the temperature program as shown below: The temperature program is as follows: Initial temperature 120℃, hold for 2 minutes, increase to 150℃ at a rate of 10℃ per minute, hold for 1 minute; increase to 154℃ at a rate of 1℃ per minute, then increase to 162℃ at a rate of 0.5℃, and finally increase to 252℃ at a rate of 20℃, hold for 2 minutes.

[0039] (3) Exclusivity.

[0040] Take the reference solution and blank solvent, analyze them according to the above detection conditions, and record the chromatograms. See the attached chromatogram for the blank solvent. Figure 1 The chromatogram of the localization solution is attached. Figure 4 The results are shown in Table 1.

[0041] Table 1: Statistical table of specificity results.

[0042]

[0043] The experimental results show that under these chromatographic conditions, anhydrous ethanol solvent does not interfere with the detection of each component in the sample, the separation degree of each component meets the requirements, and the method has good specificity.

[0044] (4) System applicability.

[0045] Take the reference solution and determine it according to the method. Inject 6 times consecutively. The results are shown in Table 2.

[0046] Table 2: Statistical table of system applicability results.

[0047]

[0048] The experimental results show that under these chromatographic conditions, the RSD of the peak area of ​​each impurity in the 6-target reference solution is less than 6%, and the RSD of the retention time is less than 1%, which meets the requirements and indicates that the system has good suitability.

[0049] (5) Limit of detection and limit of quantitation.

[0050] Limit of Quantification (LOQ) solutions: Accurately measure 1.0 mL, 1.25 mL, and 2.0 mL of 1,3-dichloropropane positioning solution, 1,7-dichloro-4-oxaheptane positioning solution, and 3-(3-chloropropoxy)prop-1-ol positioning solution, place them in a 10 mL volumetric flask, dilute to the mark with anhydrous ethanol, and shake well.

[0051] Detection limit solution: Accurately measure 2.0 mL of the quantitation limit solution, place it in a 5 mL volumetric flask, dilute to the mark with anhydrous ethanol, and shake well.

[0052] Take the limit of quantitation solution and the limit of detection solution, and determine them according to the method. The results are shown in Tables 3-4.

[0053] Table 3: Statistical table of detection limit and quantitation limit results.

[0054]

[0055] Table 4: Results of repeatability tests at the limit of quantitation.

[0056]

[0057] As can be seen from the data in Table 3, the detection method provided by the present invention has high sensitivity in detecting the purity of 3-chloro-1-propanol and its impurities, and the quantitation limit has good repeatability.

[0058] (6) Linearity and range.

[0059] Accurately weigh appropriate amounts of 3-chloro-1-propanol, 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane, and 3-(3-chloropropoxy)prop-1-ol reference standards, and prepare samples at 6 concentration levels (5 concentration levels for 3-chloro-1-propanol). Inject the above sample solutions according to the above chromatographic conditions, measure the peak area, plot the standard working curve with the concentration of the components in the sample solution as the abscissa and the peak area as the ordinate, and establish a linear equation. The final experimental results are shown in Table 5.

[0060] Table 5: Linearity test results for each component.

[0061]

[0062] Experimental results show that the detection method provided by this invention has a wide linear range, and the concentrations of 3-chloro-1-propanol and its related substances have a good linear relationship with the peak areas measured by gas chromatography.

[0063] (7) Repetitiveness.

[0064] Take the test solution (prepare 6 in parallel) and test it according to the method of the present invention. The test results are shown in Table 6.

[0065] Table 6: Statistics on repeatability results.

[0066]

[0067] The experimental results show that the detection method provided by this invention can repeatedly detect the purity of 3-chloro-1-propanol and related substances in the same batch with basically consistent results, demonstrating good repeatability.

[0068] (8) Accuracy.

[0069] Accurately weigh appropriate amounts of 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane, and 3-(3-chloropropoxy)prop-1-ol reference standards, and prepare a mixed solution with anhydrous ethanol at 10 times the limit concentration as the reference standard stock solution. Accurately measure 1.0 ml of the test solution and place it in a 10 ml volumetric flask. Prepare 9 parallel solutions, and accurately add 0.8 ml, 1.0 ml, and 1.2 ml of the reference standard stock solution to each solution. After diluting to the mark with anhydrous ethanol, use the spiked test solution for recovery. Detect the solutions using the detection method and chromatographic conditions provided in this invention. Detect each test solution in parallel 3 times. The final recovery rates of 3-chloro-1-propanol related substances are shown in Table 7.

[0070] Table 7: Recovery rate test results.

[0071]

[0072] The experimental results show that the recoveries of 9 samples of 3-chloro-1-propanol-related substances are between 90% and 110%, and the RSD of the recoveries of the 9 samples is less than 5%, which proves that the method has good accuracy.

[0073] (9) Durability test.

[0074] Take the reference solution and the test solution respectively, and change the detector temperature, injection port temperature, split ratio and flow rate respectively, while keeping other detection conditions unchanged. The final resolution and content of each substance are shown in Table 8.

[0075] Table 8: Statistical table of durability test results.

[0076]

[0077] The data in the table above show that changing the detector temperature, inlet temperature, split ratio, and flow rate resulted in a resolution greater than 1.2 for the purity of 3-chloro-1-propanol and related substances, with no significant changes in the content values, indicating that the method has good robustness.

[0078] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any simple modifications or equivalent changes made to the above embodiments based on the technical essence of the present invention shall fall within the protection scope of the present invention.

Claims

1. A method for simultaneously detecting the purity of 3-chloro-l-propanol and its impurities, characterized in that, The impurities include 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane and 3-(3-chloropropoxy)propan-1-ol, and the method comprises the following steps: S1, preparation of test sample solution: accurately weigh a proper amount of 3-chloro-1-propanol test sample, dissolve and dilute with anhydrous ethanol to obtain a test sample solution; S2, preparation of control sample solution: accurately weigh a proper amount of 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane and 3-(3-chloropropoxy)propan-1-ol control sample respectively, dissolve and dilute with anhydrous ethanol to obtain a mixed control sample solution containing three impurities; S3, gas chromatography determination: the control sample solution prepared in step S2 and the test sample solution prepared in step S1 are respectively subjected to gas chromatography detection, and the chromatogram is recorded, and the separation degree between 3-chloro-1-propanol and each impurity substance in gas chromatography separation is all ≥1.5; S4, result calculation: according to the peak area, concentration of each substance in the control sample solution and the peak area of the corresponding substance in the test sample solution, the content of 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane and 3-(3-chloropropoxy)propan-1-ol in the test sample is calculated by external standard method; at the same time, the purity of 3-chloro-1-propanol is calculated by area normalization method.

2. The method of claim 1, wherein, In step S1, the weighing amount of 3-chloro-1-propanol test sample is 0.1-1g, and the dissolving volume of anhydrous ethanol is 5-50mL.

3. The method of claim 1, wherein, In step S2, the concentration of 1,3-dichloropropane, 1,7-dichloro-4-oxaheptane and 3-(3-chloropropoxy)propan-1-ol in the mixed control sample solution is 10-30μg / mL.

4. The method of claim 1, wherein, In step S3, the detector temperature of gas chromatography detection is 200-300℃; FID flame ionization detector and polar capillary column are used for gas chromatography detection.

5. The method of claim 1, wherein, In step S3, the injection port temperature of gas chromatography detection is 100-200℃, the carrier gas flow rate is 1.0-2.0mL / min, the split ratio is 5-15:1, and the injection volume is 1-8μL.

6. The method of claim 1, wherein, In step S3, the following temperature rising conditions are used for gas chromatography detection: The initial temperature of the chromatographic column is 120℃, and maintained for 2min; The temperature is raised to 150℃ at a rate of 10℃ per minute, and maintained for 1min; After the temperature is raised to 154℃ at a rate of 1℃ per minute, the temperature is raised to 162℃ at a rate of 0.5℃ per minute; Finally, the temperature is raised to 252℃ at a rate of 20℃ per minute, and maintained for 2min.

7. The method of claim 1, wherein, In step S3, gradient elution is used for gas chromatography detection.

8. The method of claim 1, wherein, The solvents used for preparing the control sample solution and the test sample solution are all anhydrous ethanol, and the specifications of the solvents are consistent.

9. The method of claim 1, wherein: In step S4, when calculating the purity of 3-chloro-1-propanol, the calculation formula of area normalization method is: 3-chloro-1-propanol purity=(peak area of 3-chloro-1-propanol / total of all peak areas)×100%; The calculation formula for calculating 3-chloro-1-propanol impurities is: 3-chloro-1-propanol impurity content = (A 供试品 x C 对照品 ) / (A 对照品 x C 供试品 ) x 100%, wherein A 供试品 represents the test sample peak area; C 对照品 represents the control sample concentration; A 对照品 represents the control peak area; C 供试品 represents the test sample 3-chloro-l-propanol concentration.

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