Cleaning method for high performance liquid chromatography mobile phase related equipment
By using a disinfectant solution containing sodium hypochlorite and solvent, combined with ultrasonic cleaning technology, the problem of poor cleaning effect of high-performance liquid chromatography mobile phase related equipment is solved, effectively removing microorganisms and impurities, and improving the stability of equipment operation and the accuracy of analysis results.
Patent Information
- Application Number
- CN202411897900.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-23
- Publication Date
- 2025-04-15
AI Technical Summary
At this stage, the cleaning effect of high-performance liquid chromatography mobile phase-related equipment is poor, and it is especially difficult to effectively remove organic matter from the suction filter head and PTFE pipeline, resulting in blockage and inaccuracy of analysis results.
A disinfection solution prepared with sodium hypochlorite solution and solvent is used, combined with ultrasonic cleaning technology, to remove impurities and microorganisms from the parts to be cleaned. The effective chlorine content of the disinfection solution shall not be less than 5.5%, and the cleaning effect shall be improved by ultrasonic peeling off impurities with strong adhesion.
It significantly improves the cleaning effect of high-performance liquid chromatography mobile phase-related equipment, effectively removes microorganisms and strong adhesion impurities, ensures the stable operation of the equipment and the accuracy of analysis results.
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Figure CN119819640A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of detection equipment cleaning, and in particular to a cleaning method for high performance liquid chromatography mobile phase related equipment. Background Art
[0002] Liquid chromatograph is an analytical instrument widely used in the fields of chemistry, biology, medicine, etc. Its working principle is to first dissolve the sample to be tested to obtain a sample solution, then the mobile phase of the liquid reservoir is pumped into the system through a high-pressure pump, and the sample solution enters the mobile phase through an injector, and then the sample solution is loaded into the chromatographic column (stationary phase) by the mobile phase, and then the sample solution and the mobile phase are separated and detected through the chromatographic column. In the above process, the suction filter head of the mobile phase and the polytetrafluoroethylene (PTFE) material pipeline are important components in the liquid chromatograph. Their main function is not only to transport the mobile phase, but also to filter impurities and particulate matter in the mobile phase through a small diameter, preventing these impurities and particulate matter from entering the chromatographic column and affecting the separation effect. Since the mobile phase may contain a large amount of impurities and particulate matter, the suction filter head and PTFE pipeline will gradually be blocked by these impurities and fine particles during use. These blockages may reduce the flow rate of the mobile phase, and may even cause the suction filter head and PTFE pipeline to be completely blocked.
[0003] In order to solve the possible blockage problem of the suction filter head and PTFE pipeline, it is generally necessary to filter the mobile phase before use to improve the purity of the mobile phase. However, some mobile phases require to be prepared and used immediately. Filtering in advance will affect the activity of the mobile phase. Therefore, the common operation at this stage is to clean and maintain the suction filter head and PTFE pipeline after use; and the selection of different cleaning methods and different cleaning technology levels are directly related to the use effect of the instrument and the accuracy of the analysis results. However, the current cleaning method is difficult to effectively remove organic matter from the suction filter head and PTFE pipeline, resulting in poor cleaning effect of the suction filter head and PTFE pipeline. Summary of the invention
[0004] The present application provides a cleaning method for high performance liquid chromatography mobile phase related equipment to solve the following technical problem: how to improve the cleaning effect of high performance liquid chromatography mobile phase related equipment.
[0005] In a first aspect, an embodiment of the present application provides a method for cleaning a high performance liquid chromatography mobile phase-related device, the cleaning method comprising:
[0006] Disassemble the parts to be cleaned of the HPLC mobile phase related equipment;
[0007] Performing a first cleaning on the part to be cleaned to obtain a pre-cleaned part;
[0008] Mixing a sodium hypochlorite solution and a solvent to obtain a disinfectant solution; wherein the mass of effective chlorine in the sodium hypochlorite solution is greater than or equal to 5.5% of the mass of the sodium hypochlorite solution;
[0009] The pre-cleaned component is ultrasonically cleaned using the disinfection solution to remove impurities and microorganisms from the pre-cleaned component to obtain a disinfected component.
[0010] Optionally, the mass of effective chlorine in the sodium hypochlorite solution is 5.5% to 6.5% of the mass of the sodium hypochlorite solution.
[0011] Optionally, the mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent satisfy the relationship: m1:m2=1:(2.5-3.5).
[0012] Optionally, the frequency of the ultrasonic cleaning is 80kHz to 120kHz, and the time of the ultrasonic cleaning is 10min to 60min.
[0013] Optionally, the pre-cleaned component is ultrasonically cleaned using the disinfection solution to remove impurities and microorganisms from the pre-cleaned component to obtain a disinfected component, followed by the steps of:
[0014] Performing a second cleaning on the sterilized component to obtain a clean component;
[0015] The clean parts are dried to complete the cleaning of the high performance liquid chromatography mobile phase related equipment.
[0016] Optionally, the drying method includes natural air drying and / or oven drying.
[0017] Optionally, when the drying method includes oven drying, the drying temperature is 55° C. to 65° C., and the drying time is ≥30 min.
[0018] Optionally, the cleaning agent used in the second cleaning includes deionized water, and the time of the second cleaning is ≥5 min.
[0019] Optionally, the cleaning agent used in the first cleaning includes ultrapure water, and the time of the first cleaning is ≥5 min.
[0020] Optionally, the parts to be cleaned include a suction filter head and / or a polytetrafluoroethylene pipeline.
[0021] The above technical solution provided by the embodiment of the present application has the following advantages compared with the prior art:
[0022] The embodiment of the present application provides a cleaning method for high performance liquid chromatography mobile phase related equipment. The cleaning method uses a disinfection solution prepared by a sodium hypochlorite solution and a solvent. In addition, the mass of the effective chlorine in the sodium hypochlorite solution is greater than or equal to 5.5% of the mass of the sodium hypochlorite solution, so that the disinfection solution has a sufficient amount of effective chlorine component. Based on the strong oxidizing property of the effective chlorine component, the effective chlorine component can effectively oxidize the cell structure of various bacteria and viruses of the parts to be cleaned to kill these microorganisms. At the same time, sodium hypochlorite can also oxidize and reduce impurities to improve the cleaning effect of these parts to be cleaned. In addition, by ultrasonic cleaning, the ultrasonic wave of the ultrasonic cleaning can cause resonance of the parts to be cleaned, and impurities with strong adhesion of the parts to be cleaned can be stripped off to expose a large number of binding surfaces with microorganisms. A large number of binding surfaces can effectively promote the effective chlorine component of the disinfection solution to effectively bind with the microorganisms to kill these microorganisms, thereby effectively removing impurities of the parts to be cleaned and killing microorganisms of the parts to be cleaned. Therefore, the cleaning method combines the disinfection solution containing sodium hypochlorite solution with ultrasonic cleaning, which can effectively improve the cleaning effect of high performance liquid chromatography mobile phase related equipment. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and, together with the description, serve to explain the principles of the present application.
[0024] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.
[0025] Figure 1 A schematic flow chart of the main steps of a cleaning method for high performance liquid chromatography mobile phase related equipment provided in an embodiment of the present application;
[0026] Figure 2 A schematic flow chart of a cleaning method for high performance liquid chromatography mobile phase related equipment provided in an embodiment of the present application. DETAILED DESCRIPTION
[0027] In order to make the purpose, technical solution and advantages of the embodiments of the present application clearer, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application.
[0028] Various embodiments of the present application may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity and should not be understood as a rigid limitation on the scope of the present application; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single numerical values within the range; for example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which applies regardless of the range; in addition, whenever a numerical range is indicated in this document, it is meant to include any cited number (fractional or integer) within the indicated range.
[0029] In this document, the terms including "including" and "including" mean "including but not limited to". Relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. "And / or" describes the association relationship of associated objects, indicating that there can be three relationships. For example, A and / or B can mean: A exists alone, A and B exist at the same time, and B exists alone; where A and B can be singular or plural. "At least one" means one or more, and "plurality" means two or more; "at least one", "at least one of the following" or similar expressions, refers to any combination of these items, including any combination of single or plural items; for example, "at least one of a, b, or c", or "at least one of a, b, and c" can all mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple. "Parts" such as parts by weight and parts by mass indicate the proportional relationship between the components. In the proportional relationship involved in this article, the parameters that need to be described by proportion should be understood as the first term of the proportional formula in the order of description, and the proportional numbers should be understood as the second term of the proportional formula. For example, if the mass ratio of substance A, substance B and substance C is 1:2:3, then substance A, substance B and substance C should correspond to the proportional numbers in the proportional formula in the order of description, that is, the mass of substance A: the mass of substance B: the mass of substance C = 1:2:3.
[0030] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in this article can be purchased from the market or prepared by existing methods.
[0031] Figure 1A schematic flow chart of the main steps of a cleaning method for high performance liquid chromatography mobile phase related equipment provided in an embodiment of the present application is exemplarily shown;
[0032] like Figure 1 As shown, the embodiment of the present application provides a cleaning method for high performance liquid chromatography mobile phase related equipment, the cleaning method comprising:
[0033] S1. Disassemble the parts to be cleaned of the HPLC mobile phase related equipment;
[0034] S2. The component to be cleaned is first cleaned to obtain a pre-cleaned component;
[0035] S3. Mixing a sodium hypochlorite solution and a solvent to obtain a disinfectant solution; wherein the mass of available chlorine in the sodium hypochlorite solution is greater than or equal to 5.5% of the mass of the sodium hypochlorite solution;
[0036] S4. Using the disinfection solution to ultrasonically clean the pre-cleaned component to remove impurities and microorganisms from the pre-cleaned component to obtain a disinfected component.
[0037] It should be noted that the sodium hypochlorite solution can be commercially available 84 disinfectant.
[0038] It should be noted that the solvent can be deionized water or ultrapure water.
[0039] It should be noted that during the first cleaning process, larger impurities on the parts to be cleaned can be flushed out to remove dirt and residues on the parts to be cleaned.
[0040] The embodiment of the present application provides a cleaning method for high performance liquid chromatography mobile phase related equipment. The core of the cleaning method is to use a disinfection solution prepared by a sodium hypochlorite solution and a solvent, and combine it with ultrasonic cleaning technology. The specific principles are as follows: 1. The role of the disinfection solution: The disinfection solution is mixed with a sodium hypochlorite solution and a solvent, wherein the effective chlorine content of the sodium hypochlorite solution accounts for no less than 5.5%. This ratio ensures that the disinfection solution contains a sufficient amount of effective chlorine components. Since effective chlorine has strong oxidizing properties, it can oxidize the cell structure of microorganisms such as bacteria and viruses on the parts to be cleaned, thereby killing these microorganisms. At the same time, sodium hypochlorite can also oxidize and reduce impurities, further improving the cleaning effect.
[0041] 2. Synergistic effect of ultrasonic cleaning: Ultrasonic cleaning uses the vibration of ultrasonic waves to remove impurities (including organic matter, inorganic salts and other impurities) with strong adhesion on the parts to be cleaned. In this way, the binding surface originally covered by impurities is exposed, providing more opportunities for the effective chlorine components of the disinfectant solution to bind with microorganisms. In addition, a large number of binding surfaces allow the effective chlorine components to bind with microorganisms more effectively, thereby killing these microorganisms. The synergistic effect of ultrasonic cleaning and disinfectant solutions greatly improves the efficiency of cleaning and disinfection.
[0042] In summary, the embodiment of the present application provides a cleaning method for high performance liquid chromatography mobile phase related equipment. The cleaning method, through the combination of a disinfectant solution containing sodium hypochlorite and ultrasonic cleaning technology, can not only effectively kill microorganisms on the parts to be cleaned, but also completely remove impurities with strong adhesion, thereby significantly improving the cleaning effect of high performance liquid chromatography mobile phase related equipment.
[0043] In some optional embodiments, the mass of available chlorine in the sodium hypochlorite solution is 5.5% to 6.5% of the mass of the sodium hypochlorite solution;
[0044] In these embodiments, the mass of the effective chlorine in the sodium hypochlorite solution can be 5.5% to 6.5% of the mass of the sodium hypochlorite solution, so that the sodium hypochlorite solution has sufficient effective chlorine. Sufficient effective chlorine can effectively kill microorganisms. In addition, sufficient effective chlorine can also oxidize and reduce impurities to improve the cleaning effect of the parts to be cleaned.
[0045] The mass of available chlorine in the sodium hypochlorite solution may be 5.5%, 5.6%, 5.7%, 5.8%, 5.9%, 6.0%, 6.1%, 6.2%, 6.3%, 6.4% or 6.5% of the mass of the sodium hypochlorite solution.
[0046] In some optional embodiments, the mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent satisfy the relationship: m1:m2=1:(2.5-3.5);
[0047] In these embodiments, the mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent can satisfy the relationship: m1:m2=1:(2.5-3.5), so that the sodium hypochlorite solution and the solvent are fully mixed and a sufficient amount of effective chlorine components such as hypochlorous acid are formed, which is convenient for the subsequent effective killing of microorganisms and redox impurities.
[0048] The mass m2 of the solvent can be 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, 3.3, 3.4 or 3.5.
[0049] In some optional embodiments, the frequency of the ultrasonic cleaning is 80kHz to 120kHz, and the time of the ultrasonic cleaning is 10min to 60min;
[0050] In these embodiments, the frequency of ultrasonic cleaning can be 80kHz to 120kHz, and the time of ultrasonic cleaning can be 10min to 60min, so that ultrasonic cleaning has sufficient frequency and time. Ultrasonic cleaning with sufficient frequency and time can effectively expose a large number of binding surfaces with microorganisms, and a large number of binding surfaces can effectively promote the effective chlorine component of the disinfectant solution to effectively combine with the microorganisms, which can improve the microbial killing effect of the disinfectant solution, thereby effectively removing impurities in the parts to be cleaned and killing the microorganisms in the parts to be cleaned.
[0051] The frequency of the ultrasonic cleaning may be 80 kHz, 85 kHz, 90 kHz, 95 kHz, 100 kHz, 105 kHz, 110 kHz, 115 kHz or 120 kHz.
[0052] The ultrasonic cleaning time can be 10 min, 15 min, 20 min, 25 min, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min or 60 min.
[0053] Figure 2 A schematic flow chart of a cleaning method for high performance liquid chromatography mobile phase related equipment provided in an embodiment of the present application is exemplarily shown;
[0054] In some optional embodiments, such as Figure 2 As shown, the method uses the disinfection solution to ultrasonically clean the pre-cleaned component to remove impurities and microorganisms from the pre-cleaned component to obtain a disinfected component, and then includes the steps of:
[0055] S5. The disinfected component is subjected to a second cleaning to obtain a pure component;
[0056] S6. Drying the clean parts to complete the cleaning of the HPLC mobile phase-related equipment;
[0057] In these embodiments, the disinfection component is subjected to a second cleaning to remove the residual disinfection solution and attached impurities from the disinfection component to obtain a pure component, and then the moisture in the pure component is removed by drying, thereby completing the cleaning of the HPLC mobile phase-related equipment.
[0058] It should be noted that after the cleaning of the HPLC mobile phase related equipment is completed, the cleaning effect can be evaluated by visual inspection, water flow test, weight comparison and other methods to ensure that microorganisms, organic matter, inorganic salts and other impurities have been completely removed.
[0059] In addition, before reinstalling the mobile phase related equipment, you need to carefully check the cleaning status of the HPLC mobile phase related equipment to ensure that the surface of these equipment is clean and has no scratches, damage or deformation. Then, according to the instructions in the instrument manual, install these cleaned and checked equipment on the liquid chromatograph to ensure that these equipment are correctly installed and fully tightened, then restart the liquid chromatograph and perform a functional test. Observe the working status of these equipment to ensure that there are no leaks, blockages, etc. If there are any abnormalities, you need to recheck the installation and cleaning steps of these equipment.
[0060] In some optional embodiments, the drying method includes natural air drying and / or oven drying;
[0061] In these embodiments, the drying method may include natural air-drying and / or baking, and the moisture of the pure parts can be removed by drying to complete the cleaning of the high performance liquid chromatography mobile phase related equipment.
[0062] In some optional embodiments, when the drying method includes drying, the drying temperature is 55° C. to 65° C., and the drying time is ≥ 30 min;
[0063] In these embodiments, when the drying method includes baking, the drying temperature can be 55°C to 65°C, and the drying time can be ≥30 minutes. The drying method can effectively remove the moisture from the pure parts to complete the cleaning of the high performance liquid chromatography mobile phase related equipment.
[0064] The drying temperature can be 55°C, 56°C, 57°C, 58°C, 59°C, 60°C, 61°C, 62°C, 63°C, 64°C or 65°C.
[0065] The drying time can be 30 min, 35 min, 40 min, 45 min, 50 min, 55 min or 60 min.
[0066] In some optional embodiments, the cleaning agent used in the second cleaning includes deionized water, and the time of the second cleaning is ≥5 min;
[0067] In these embodiments, the cleaning agent used in the second cleaning may include deionized water, and the second cleaning time is ≥5 minutes, so that the second cleaning can effectively remove the residual disinfectant and attached impurities on the disinfected component to obtain a pure component.
[0068] The second cleaning time can be 5 min, 10 min, 15 min, 20 min, 25 min or 30 min.
[0069] In some optional embodiments, the cleaning agent used in the first cleaning includes ultrapure water, and the time of the first cleaning is ≥5 min;
[0070] In these embodiments, the cleaning agent used for the first cleaning may include ultrapure water, and the time for the first cleaning may be ≥5 minutes. The first cleaning method can fully remove impurities such as attachments and dirt on the parts to be cleaned to obtain relatively pure pre-cleaned parts, which is convenient for subsequent ultrasonic cleaning of the pre-cleaned parts with a disinfectant.
[0071] The first cleaning time can be 5 min, 10 min, 15 min, 20 min, 25 min or 30 min.
[0072] In some optional embodiments, the parts to be cleaned include suction filters and / or polytetrafluoroethylene pipelines;
[0073] In these embodiments, the parts to be cleaned may include suction filters and / or polytetrafluoroethylene pipes, and may cover mobile phase-related equipment of high performance liquid chromatography to achieve effective cleaning of mobile phase-related equipment of high performance liquid chromatography.
[0074] It should be noted that the parts to be cleaned, in addition to the suction filter head and the polytetrafluoroethylene pipe, may also be rubber pads related to the mobile phase.
[0075] The present application is further described below in conjunction with specific examples. The experimental methods in the following examples where specific conditions are not specified are usually measured in accordance with national standards / industry standards; if there are no corresponding national standards / industry standards, they are measured in accordance with common international standards, conventional conditions or conditions recommended by the manufacturer.
[0076] Example 1
[0077] like Figure 1 As shown, a cleaning method for high performance liquid chromatography mobile phase related equipment comprises:
[0078] S1. Disassemble the parts to be cleaned of the HPLC mobile phase related equipment;
[0079] S2. The parts to be cleaned are first cleaned to obtain pre-cleaned parts;
[0080] S3. Mixing a sodium hypochlorite solution (84 disinfectant) and a solvent to obtain a disinfectant solution; wherein the mass of available chlorine in the sodium hypochlorite solution is greater than or equal to 5.5% of the mass of the sodium hypochlorite solution;
[0081] S4. Ultrasonic cleaning of the pre-cleaned parts using a disinfecting solution to remove impurities and microorganisms from the pre-cleaned parts to obtain disinfected parts;
[0082] S5. The sterilized parts are cleaned for a second time to obtain pure parts;
[0083] S6. Dry the clean parts to complete the cleaning of the HPLC mobile phase related equipment.
[0084] The mass of available chlorine in the sodium hypochlorite solution is 6.0% of the mass of the sodium hypochlorite solution.
[0085] The mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent satisfy the relationship: m1:m2=1:3.0.
[0086] The frequency of ultrasonic cleaning is 100 kHz, and the time of ultrasonic cleaning is 40 min.
[0087] The drying method is natural drying.
[0088] The cleaning agent used in the second cleaning includes deionized water, and the second cleaning time is 5 minutes.
[0089] The cleaning agent used in the first cleaning includes ultrapure water, and the first cleaning time is 5 minutes.
[0090] Example 2
[0091] Based on the contents disclosed in Example 1, the following modifications are further made:
[0092] The mass of available chlorine in the sodium hypochlorite solution is 5.5% of the mass of the sodium hypochlorite solution.
[0093] The mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent satisfy the relationship: m1:m2=1:2.5.
[0094] The frequency of ultrasonic cleaning is 80kHz, and the time of ultrasonic cleaning is 60min.
[0095] Example 3
[0096] Based on the contents disclosed in Example 1, the following modifications are further made:
[0097] The mass of available chlorine in the sodium hypochlorite solution is 6.5% of the mass of the sodium hypochlorite solution.
[0098] The mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent satisfy the relationship: m1:m2=1:3.5.
[0099] The frequency of ultrasonic cleaning is 120kHz, and the time of ultrasonic cleaning is 10min.
[0100] Example 4
[0101] Based on the contents disclosed in Example 1, the following modifications are further made:
[0102] The drying method is drying.
[0103] When the drying method includes drying, the drying temperature is 60° C. and the drying time is 40 minutes.
[0104] Comparative Example 1
[0105] Based on the contents disclosed in Example 1, the following modifications are further made:
[0106] Do not use a solution containing sodium hypochlorite; instead, use an equal amount of anhydrous ethanol directly.
[0107] Comparative Example 2
[0108] Based on the contents disclosed in Example 1, the following modifications are further made:
[0109] Instead of ultrasonic cleaning, stirring cleaning was performed directly. The speed of stirring cleaning was 200 r / min, and the time of stirring cleaning was 40 min.
[0110] Comparative Example 3
[0111] Based on the contents disclosed in Example 1, the following modifications are further made:
[0112] The mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent satisfy the relationship: m1:m2=1:1.5.
[0113] Comparative Example 4
[0114] Based on the contents disclosed in Example 1, the following modifications are further made:
[0115] The mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent satisfy the relationship: m1:m2=1:4.5.
[0116] Comparative Example 5
[0117] Based on the contents disclosed in Example 1, the following modifications are further made:
[0118] The frequency of ultrasonic cleaning is 60kHz, and the time of ultrasonic cleaning is 70min.
[0119] Comparative Example 6
[0120] Based on the contents disclosed in Example 1, the following modifications are further made:
[0121] The frequency of ultrasonic cleaning is 140kHz, and the time of ultrasonic cleaning is 5min.
[0122] Related experiments and effect data:
[0123] The cleaning liquid obtained by the second cleaning of each embodiment and comparative example was collected respectively, and the cleaning liquid was used as the test sample, inoculated into multiple complete culture media for culture, and the average number of colonies in these complete culture media was counted. The results are shown in Table 1; in addition, the high performance liquid chromatography mobile phase related equipment after cleaning was subjected to visual inspection, water flow test, weight comparison and other methods in turn to judge whether the cleaning process was qualified, and the results are shown in Table 1.
[0124] Table 1 Cleaning effect results of various embodiments and comparative examples
[0125]
[0126] It can be seen from Table 1 that the colonies of the cleaning solutions in each embodiment are relatively small, and the cleaning process is judged to be qualified, which shows that the cleaning method provided in the embodiments of the present application can effectively kill the microorganisms on the parts to be cleaned.
[0127] In addition, comparative example 1 uses anhydrous ethanol, and its microbial killing effect is poor; in addition, although the microbial killing effect of comparative example 2 is the same as that of the embodiment, due to the use of stirring cleaning, the cleaning effect is poor; in addition, the concentration of the sodium hypochlorite component of the disinfectant solution used in comparative example 3 is low, resulting in a poor sterilization effect; in addition, comparative example 4 uses an excessive amount of sodium hypochlorite component, which will cause part of the disinfectant to remain in the high-performance liquid chromatography mobile phase-related equipment and is difficult to be cleaned; in addition, comparative examples 5 and 6 use a lower ultrasonic cleaning frequency and a higher ultrasonic cleaning frequency, respectively. The lower ultrasonic cleaning frequency cannot effectively remove impurities from the pre-cleaning components and promote the killing effect of the disinfectant, resulting in a poor final cleaning effect; and the higher ultrasonic cleaning frequency not only causes ultrasonic cleaning to require a large amount of energy consumption, but may also cause damage to the pre-cleaning components.
[0128] In summary, the embodiment of the present application provides a cleaning method for high performance liquid chromatography mobile phase related equipment. The cleaning method, through the combination of a disinfectant solution containing sodium hypochlorite and ultrasonic cleaning technology, can not only effectively kill microorganisms on the parts to be cleaned, but also completely remove impurities with strong adhesion, thereby significantly improving the cleaning effect of high performance liquid chromatography mobile phase related equipment.
[0129] In addition, an embodiment of the present application provides a cleaning method for HPLC mobile phase related equipment. The HPLC mobile phase related equipment cleaned by the cleaning method can operate stably in the subsequent use stage, and can improve the accuracy and reliability of the HPLC analysis process.
[0130] The above description is only a specific implementation of the present application, so that those skilled in the art can understand or implement the present application. It will be apparent to those skilled in the art that various modifications to these embodiments are possible, and the general principles defined in the present application can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown in the present application, but will conform to the widest range consistent with the principles and novel features applied for by the present application.
Claims
1. A cleaning method for high performance liquid chromatography mobile phase related equipment, the cleaning method comprising: Disassemble the parts to be cleaned of the HPLC mobile phase related equipment; Performing a first cleaning on the part to be cleaned to obtain a pre-cleaned part; Mixing a sodium hypochlorite solution and a solvent to obtain a disinfectant solution; wherein the mass of effective chlorine in the sodium hypochlorite solution is greater than or equal to 5.5% of the mass of the sodium hypochlorite solution; The pre-cleaned component is ultrasonically cleaned using the disinfection solution to remove impurities and microorganisms from the pre-cleaned component to obtain a disinfected component.
2. The cleaning method according to claim 1, wherein the mass of available chlorine in the sodium hypochlorite solution is 5.5% to 6.5% of the mass of the sodium hypochlorite solution.
3. The cleaning method according to claim 1 or 2, wherein the mass m1 of the sodium hypochlorite solution and the mass m2 of the solvent satisfy the relationship: m1:m2=1:(2.5-3.5). 4 . The cleaning method according to claim 1 , wherein the frequency of the ultrasonic cleaning is 80 kHz to 120 kHz, and the time of the ultrasonic cleaning is 10 min to 60 min.
5. The cleaning method according to claim 1, wherein the pre-cleaned component is ultrasonically cleaned using the disinfection solution to remove impurities and microorganisms from the pre-cleaned component to obtain a disinfected component, and then comprises the steps of: Performing a second cleaning on the sterilized component to obtain a clean component; The clean parts are dried to complete the cleaning of the high performance liquid chromatography mobile phase related equipment.
6. The cleaning method according to claim 5, wherein the drying method comprises natural air drying and / or oven drying.
7. The cleaning method according to claim 6, when the drying method includes drying, the drying temperature is 55°C to 65°C, and the drying time is ≥30 minutes. 8 . The cleaning method according to claim 5 , wherein the cleaning agent used in the second cleaning comprises deionized water, and the time of the second cleaning is ≥5 min. 9 . The cleaning method according to claim 1 , wherein the cleaning agent used in the first cleaning comprises ultrapure water, and the time of the first cleaning is ≥5 min.
10. The cleaning method according to claim 1, wherein the parts to be cleaned include a suction filter head and / or a polytetrafluoroethylene pipeline.
Citation Information
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