CN118311167A - Acceptance method for metronidazole and chloramphenicol mass spectrum detection water - Google Patents
Acceptance method for metronidazole and chloramphenicol mass spectrum detection water Download PDFInfo
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- CN118311167A CN118311167A CN202410432194.6A CN202410432194A CN118311167A CN 118311167 A CN118311167 A CN 118311167A CN 202410432194 A CN202410432194 A CN 202410432194A CN 118311167 A CN118311167 A CN 118311167A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/02—Column chromatography
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Abstract
The invention provides an acceptance method for water for mass spectrometry detection of metronidazole and chloramphenicol, belonging to the technical field of drug detection. A method for checking and accepting water for detecting metronidazole and chloramphenicol mass spectrum comprises a series of steps of visual observation, accurate measurement, preparation of reference substance solution, determination of detection limit, determination of water sample applicability and the like; according to the invention, by means of refining and expanding the mass requirements of the water for mass spectrometry detection, establishing an acceptance method of specific substances, introducing blank solution contrast experiments and the like, on one hand, the water for mass spectrometry detection is more comprehensive on the basis of the existing acceptance standard, and the quality monitoring is more perfect; on the other hand, the deviation of results caused by the wrong selection of the experimental water is effectively prevented, in addition, the method shows good linear relation, the blank solution is free from interference, and the actually measured minimum detected concentration is lower than the minimum detected concentration limit value set by the method, so that more reliable and effective technical support is provided for mass spectrum detection in the fields of cosmetics, foods, medicines and the like.
Description
Technical Field
The invention relates to the technical field of medicine detection, in particular to an acceptance method for water for mass spectrum detection of metronidazole and chloramphenicol.
Background
Metronidazole and chloramphenicol are antibiotic forbidden substances in cosmetics, are often illegally added into acne and mite removing products, and are easy to cause symptoms such as contact dermatitis and allergy after long-term use, and are easy to generate drug resistance. As a key project for risk monitoring in cosmetics, the general detection method is high performance liquid chromatography tandem mass spectrometry specified in chapter 2.35 of cosmetic safety technical Specification (2015 edition). Mass spectrometry is a highly sensitive analytical technique that can be used to achieve trace analysis, with water levels typically being ultrapure water or laboratory grade or high purity water. Laboratories typically use specialized water treatment systems to prepare water for mass spectrometry. These systems include deionized water machines, distilled water machines, ultra-pure water machines, etc., which can ensure the purity, stability, and consistency of water.
In the actual detection process of metronidazole and chloramphenicol, the following steps are found: the method is characterized in that when water prepared by an ultra-pure water machine accepted by national standards is taken and used as experimental water, a mass spectrum peak cannot be detected, the water is changed into self-purchased distilled water and then the peak is normally generated, so that the selection of the experimental water influences whether the Metronidazole and the chloramphenicol can normally generate the peak, the reliability of the detection result is concerned, the current general acceptance standards of the laboratory water include GB/T6682-2008 analytical laboratory water specification and test method, GB/T33087-2016 instrument analytical high purity water specification and test method, GB 17323-1998 bottled drinking purified water and the like, and the experimental water meeting the general acceptance standards cannot be ensured to be suitable for the determination of Metronidazole and chloramphenicol in cosmetics. Therefore, in order to solve the problem, the invention provides a method for checking and accepting water for detecting the mass spectrum of the metronidazole and the chloramphenicol, and the detection interference on a target object is eliminated by screening proper experimental water from a source head.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art, and provide an acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol, which can overcome the problems or at least partially solve the problems.
In order to solve the technical problems, the invention adopts the basic conception of the technical scheme that: a method for checking and accepting water for detecting metronidazole and chloramphenicol by mass spectrometry comprises the following steps: s1, visually observing a water sample to ensure that the water sample is colorless and transparent and has no peculiar smell so as to preliminarily judge the quality of the water sample; s2, in a clean environment, measuring by using a high performance liquid chromatography-triple quadrupole mass spectrometer, wherein: selecting a water-resistant chromatographic column; an aqueous solution for mass spectrometry containing 0.1% formic acid and a methanol solution containing 0.1% formic acid were used as mobile phase a and mobile phase B, respectively; preparing a reference substance stock solution by taking methanol as a solvent; preparing a reference substance solution and a blank solution by taking an acetonitrile solution containing 0.5% formic acid as a diluent; s3, preparing a reference substance solution, wherein the reference substance solution comprises a mixed standard series solution of metronidazole and chloramphenicol, and the mixed standard series solution is used for determining a detection limit and drawing a standard curve; s4, observing the peak-to-peak condition of chromatographic peaks by measuring a reference substance solution and a blank solution, and determining the detection limit of metronidazole and chloramphenicol; s5, replacing the surface water sample as a sample solution to be measured, and judging that the water sample is suitable for mass spectrum detection of metronidazole and chloramphenicol if the chromatographic peak areas of the blank solution and the sample solution are smaller than the actually measured minimum detection concentration.
Preferably, in step S2, the measurement conditions of the high performance liquid chromatography-triple quadrupole mass spectrometer include specific liquid phase conditions and mass spectrometry conditions, and are used for precisely measuring the content of metronidazole and chloramphenicol.
Preferably, in the step S3, when the standard curve is fitted, the concentration is taken as an abscissa, the quantitative ion chromatographic peak area is taken as an ordinate, and the linear correlation coefficient r is required to satisfy r more than or equal to 0.99.
Preferably, in step S3, the preparation of the mixed standard series solution includes: s31, precisely weighing 10mg of metronidazole and 10mg of chloramphenicol reference substances respectively, putting the metronidazole and the chloramphenicol reference substances into a 100mL volumetric flask, adding a solvent for dissolution and fixing the volume, and then mixing to obtain a standard stock solution with the mass concentration of 0.1 mg/mL; s32, precisely transferring 1ml of the mixed standard stock solution into a 100ml volumetric flask, diluting with a solvent, fixing the volume to a scale, and preparing mixed standard series solutions with different concentrations by using a diluent for subsequent quantitative analysis.
Preferably, in step S32, the standard series solutions are mixed to prepare mixed standard series solutions with different concentrations of S1 (2 ng/mL), S2 (5 ng/mL), S3 (20 ng/mL), S4 (60 ng/mL) and S5 (100 ng/mL) in sequence.
Preferably, in step S5, the process for determining the lowest detected concentration includes: s51, respectively and precisely transferring a proper amount of mixed standard working solution S1 (2 ng/mL), and diluting with a diluent until the signal to noise ratio S/N of the metronidazole and chloramphenicol peak heights reaches 3:1, namely, respectively obtaining detection limit solutions; s52, calculating to obtain the measured lowest detected concentration based on the sampling amount of 0.2 g.
Preferably, in step S52, the calculation formula of the measured lowest detected concentration includes: And in the subsequent measurement process, 2 mu L of mixed standard working solution S3 (20 ng/mL) is sampled, the mixed standard working solution S3 is injected into a high performance liquid chromatography-triple quadrupole mass spectrometer to observe whether the peak is normal, and if the peak is normal, 2 mu L of standard series solution, detection limiting solution, blank solution and sample solution are respectively sampled, wherein in the process, the chromatographic peak areas of the blank solution and the sample solution are smaller than the calculated measured minimum detection concentration.
Preferably, in step S52, the measured minimum detected concentration should meet the requirement of +.0.1 μg/g.
Preferably, the representative water sample in step S5 is ultrapure water or distilled water.
Preferably, the water sample is suitable for mass spectrometry detection of metronidazole and chloramphenicol in cosmetics such as creams, emulsions, water aquas and the like.
After the technical scheme is adopted, compared with the prior art, the invention has the following beneficial effects: according to the invention, by means of refining and expanding the mass requirements of the water for mass spectrometry detection, establishing an acceptance method of specific substances, introducing blank solution contrast experiments and the like, on one hand, the water for mass spectrometry detection is more comprehensive on the basis of the existing acceptance standard, and the quality monitoring is more perfect; on the other hand, the deviation of results caused by the wrong selection of the experimental water is effectively prevented, in addition, the method shows good linear relation, the blank solution is free from interference, and the actually measured minimum detected concentration is lower than the minimum detected concentration limit value set by the method, so that more reliable and effective technical support is provided for mass spectrum detection in the fields of cosmetics, foods, medicines and the like.
Drawings
FIG. 1 is a total ion flow chromatogram of metronidazole in a control solution of an acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol;
FIG. 2 is a qualitative ion chromatogram of metronidazole in a control solution of an acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol;
FIG. 3 is a quantitative ion flow chromatogram of metronidazole in a control solution of the acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol;
FIG. 4 is a total ion flow chromatogram of chloramphenicol in a control solution of the method for checking and accepting metronidazole and chloramphenicol mass spectrum detection water;
FIG. 5 is a qualitative ion flow chromatogram of chloramphenicol in a control solution of the method for detecting water for mass spectrometry of metronidazole and chloramphenicol;
FIG. 6 is a graph of a quantitative ion flow chromatogram of chloramphenicol in a control solution of an acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol;
FIG. 7 is a total ion flow chromatogram of metronidazole in a sample solution (distilled water) for an acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol;
FIG. 8 is a total ion flow chromatogram of chloramphenicol in a sample solution (distilled water) for use in the method for detecting water for mass spectrometry of metronidazole and chloramphenicol;
FIG. 9 is a graph of total ion flow of metronidazole in a blank solution for an acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol;
FIG. 10 is a graphic diagram of total ion flow of chloramphenicol in a blank solution for an acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol;
FIG. 11 is a mass spectrum of metronidazole in a control solution of the method for checking and accepting water for mass spectrometry of metronidazole and chloramphenicol;
FIG. 12 is a chloromycetin mass spectrum of a control solution of an acceptance method of water for metronidazole and chloromycetin mass spectrum detection provided by the invention;
FIG. 13 is a graph showing total ion flow of metronidazole in a sample solution (ultrapure water) for use in the method for detecting water for mass spectrometry of metronidazole and chloramphenicol;
FIG. 14 is a graph showing total ion flow of chloramphenicol in a sample solution (ultrapure water) for use in the method for detecting water for mass spectrometry of Metronidazole and chloramphenicol according to the present invention;
FIG. 15 is a metronidazole standard curve of an acceptance method of water for mass spectrometry detection of metronidazole and chloramphenicol provided by the invention;
fig. 16 is a chloramphenicol standard curve of the method for checking and accepting metronidazole and chloramphenicol mass spectrum detection water provided by the invention.
FIG. 17 is a solution ion flow chromatogram of metronidazole detection limit of the method for checking and accepting water for mass spectrometry detection of metronidazole and chloramphenicol;
fig. 18 is a chloramphenicol detection limit solution ion flow chromatogram of the method for checking and accepting metronidazole and chloramphenicol mass spectrometry detection water provided by the invention.
Detailed Description
The present invention is described in further detail below with reference to the drawings and examples to enable those skilled in the art to practice the invention by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
In the description of the present invention, the terms "transverse", "longitudinal", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus are not to be construed as limiting the present invention.
Referring to fig. 1-18, a method for checking and accepting metronidazole and chloramphenicol mass spectrum detection water comprises the following steps: s1, visually observing a water sample to ensure that the water sample is colorless and transparent and has no peculiar smell so as to preliminarily judge the quality of the water sample; s2, in a clean environment, measuring by using a high performance liquid chromatography-triple quadrupole mass spectrometer, wherein: selecting a water-resistant chromatographic column; an aqueous solution for mass spectrometry containing 0.1% formic acid and a methanol solution containing 0.1% formic acid were used as mobile phase a and mobile phase B, respectively; preparing a reference substance stock solution by taking methanol as a solvent; preparing a reference substance solution and a blank solution by taking an acetonitrile solution containing 0.5% formic acid as a diluent; s3, preparing a reference substance solution, wherein the reference substance solution comprises a mixed standard series solution of metronidazole and chloramphenicol, the mixed standard series solution is used for determining a detection limit and drawing a standard curve, when the standard curve is fitted, the concentration is used as an abscissa, the quantitative ion chromatographic peak area is used as an ordinate, and the linear correlation coefficient r is more than or equal to 0.99; s4, observing the peak-to-peak condition of chromatographic peaks by measuring a reference substance solution and a blank solution, and determining the detection limit of metronidazole and chloramphenicol; s5, taking a representative water sample of ultrapure water or distilled water as a sample solution to be measured, and judging that the water sample is suitable for mass spectrometry detection of metronidazole and chloramphenicol if the chromatographic peak areas of the blank solution and the sample solution are smaller than the actually measured minimum detection concentration.
In the technical scheme, the method realizes the comprehensive acceptance of the water for the mass spectrum detection of the metronidazole and the chloramphenicol and the establishment of a specific acceptance method through a series of steps of visual observation, accurate measurement, preparation of a reference substance solution, determination of the detection limit, determination of the applicability of a water sample and the like, and the method not only enriches the content of the existing acceptance standard and improves the quality monitoring perfection, but also provides a more reliable and effective water screening means for mass spectrum detection in the fields of cosmetics, foods, medicines and the like.
For the above technical solution, the matters to be noted include:
Sensory requirements: the water sample must be a colorless transparent liquid, any color or turbidity may mean that the water sample contains impurities or pollutants, and the water sample is confirmed to be odorless by means of sniffing and sniffing, so as to eliminate possible chemical residues or peculiar smell and cause interference to mass spectrum detection.
And (3) storing: the water sample should be opened immediately to ensure its freshness and avoid the pollution that may be introduced in the air of long-time exposure, and the water sample life after unsealing must not exceed 3 days, beyond this time, the water sample can receive external environment's pollution, influences the accuracy of testing result, and ultrapure water is just taken and is just used, means that ultrapure water should be obtained immediately before using, avoids long-time storage.
Sampling: before sampling, the container must be repeatedly cleaned with water to be tested to remove any residues or contaminants in the container, avoiding contamination of the water sample, taking special care during sampling, avoiding contamination, as any external contamination may affect the final detection result, the water sample should be filled into the container to ensure sufficient sampling amount, and the contact area between air in the container and the water sample is reduced, thereby reducing possible contamination.
Inspection environment: the test is performed in a clean environment, so as to ensure that the water sample is not disturbed by dust, microorganisms or other pollutants in the environment in the detection process, and proper measures are taken to avoid contamination of the sample. This may include the use of clean tools and containers, wearing clean laboratory clothing, maintaining cleanliness within the laboratory, and the like.
In a specific embodiment, in step S2, the measurement conditions of the high performance liquid chromatography-triple quadrupole mass spectrometer include specific liquid phase conditions and mass spectrometry conditions for accurately measuring the content of metronidazole and chloramphenicol.
According to the technical scheme, in terms of liquid phase conditions, a HSS T3 chromatographic column with the length of 100mm and the inner diameter of 2.1mm is selected to ensure high-efficiency separation, a mobile phase comprises water containing 0.1% formic acid (mobile phase A) and methanol containing 0.1% formic acid (mobile phase B), mixing of different proportions is realized through a gradient elution program, the elution program is gradually adjusted to 62% of the mobile phase A and 38% of the mobile phase B from the initial 85% of the mobile phase A and 15% of the mobile phase B, then is transited to 5% of the mobile phase A and 95% of the mobile phase B and finally returns to the initial proportion, the column temperature is set to 40 ℃, the sample introduction amount is 2 mu L, the flow rate is controlled to be 0.3mL/min, and the mobile phase gradient elution program is shown in Table 1.
TABLE 1 gradient elution procedure for mobile phases
In the aspect of mass spectrometry conditions, an electrospray ion source (ESI) is adopted as an ion source, positive and negative ion scanning modes are set to adapt to detection requirements of different substances, multiple Reaction Monitoring (MRM) is selected in a detection mode, so that the detection sensitivity and specificity are improved, parameters such as ionization voltage, ion source temperature, atomizing air flow, heating air flow and drying air flow are optimized, ionization efficiency and stability of mass spectrometry signals are ensured, and condition parameters of metronidazole and chloramphenicol mass spectrometry are shown in Table 2.
TABLE 2 Mass Spectrometry parameters for Metronidazole and Chloramphenicol determination
For mass spectrometry of metronidazole and chloramphenicol, respectively setting corresponding ionization mode, parent ion, child ion and Collision Energy (CE), wherein the metronidazole adopts an ESI + ionization mode, the parent ion is 172.0m/z, the quantitative ion is 82.0m/z, the qualitative ion is 128.0m/z, and the collision energy is-27V and-17V respectively; the chloramphenicol adopts an ESI - ionization mode, the parent ion is 321.1m/z, the quantitative ion is 152.0m/z, the qualitative ion is 257.2m/z, the collision energy is 16V and 11V respectively, and the selection of the parameters is based on the characteristics of the substances and the performance of the instrument, so that the best mass spectrum signal and detection effect are obtained.
In a preferred embodiment, in step S3, the preparation of the mixed standard series of solutions comprises: s31, precisely weighing 10mg of metronidazole and 10mg of chloramphenicol reference substances respectively, putting the metronidazole and the chloramphenicol reference substances into a 100mL volumetric flask, adding a solvent for dissolution and fixing the volume, and then mixing to obtain a standard stock solution with the mass concentration of 0.1 mg/mL; s32, precisely transferring 1mL of mixed standard stock solution into a 100mL volumetric flask, diluting with a solvent, fixing the volume to a scale, and preparing mixed standard series solutions with different concentrations of S1 (2 ng/mL), S2 (5 ng/mL), S3 (20 ng/mL), S4 (60 ng/mL) and S5 (100 ng/mL) by using a diluent in sequence for subsequent quantitative analysis, wherein the preparation of the mixed standard series solutions is shown in Table 3.
Table 3 mixed standard series solutions
In a process for determining a minimum detected concentration, comprising:
S51, respectively and precisely transferring a proper amount of mixed standard working solution S1 (2 ng/mL), and diluting with a diluent until the signal to noise ratio S/N of the metronidazole and chloramphenicol peak heights reaches 3:1, namely, respectively obtaining detection limit solutions;
S52, calculating the measured lowest detected concentration based on the sampling amount of 0.2g, wherein in the step S52, a calculation formula of the measured lowest detected concentration comprises:
And V is the volume of a fixed sample, the unit is milliliter, D is the dilution multiple, if not diluted, 1 is the sampling quantity, and 0.2g is taken as the sampling quantity, 2 mu L of mixed standard working solution S3 (20 ng/mL) is sampled in the subsequent measuring process, the mixed standard working solution S3 is injected into a high performance liquid chromatography-triple quadrupole mass spectrometry combined instrument, whether the peak is normal or not is observed, if the peak is normal, 2 mu L of standard series solution, detection limiting solution, blank solution and sample solution are respectively sampled, and in the process, the chromatographic peak areas of the blank solution and the sample solution are ensured to be smaller than the calculated actual measurement minimum detection concentration.
For the scheme, laboratory ultrapure water (containing 0.1% formic acid) is used as a mobile phase A in the measurement process, a mass spectrum peak is not detected by the metronidazole and chloramphenicol mixed standard working solution S3 (20 ng/mL), the mass spectrum peak is not detected through inspection, the peak is normal by using self-purchased distilled water (containing 0.1% formic acid) as the mobile phase A, the metronidazole and chloramphenicol mixed standard working solution S3 (20 ng/mL), the linearity of the standard series solution is good, the correlation coefficient is equal to 0.99, the metronidazole peak high signal to noise ratio S/N (0.2 ng/mL) is obtained by diluting the standard working solution S1 (2 ng/mL) by 10 times, the chloramphenicol peak high signal to noise ratio S/N (0.5 ng/mL) is obtained by diluting the standard working solution S1 (2 ng/mL) by 4 times (0.01 mug/g), the measured minimum detected concentration of the chloramphenicol is 0.025 mug/g, the measured minimum detected concentration of the chloramphenicol is equal to <0.1 mug/g, the average value is equal to <0.1 mug/g, the correlation coefficient is equal to 18, and the ion graph is represented by a graph with a blank time, and the graph is represented by the graph with the ion graph and the average time is represented by the graph and the graph is represented by the vertical time.
It is further described that, the invention further refines and expands the quality requirement of water for mass spectrometry detection based on following national standard GB/T33087-2016 high purity water specification and test method for instrument analysis, especially for conductivity, total Organic Carbon (TOC) and non-conventional matter percentage, the invention sets a stricter limit value to ensure that the water quality reaches the ultra-high purity water requirement, so that even if the experimental water meets the national standard, the invention can further screen high purity water more meeting the mass spectrometry detection requirement by the acceptance method, thereby improving the accuracy and reliability of the detection result, and secondly, in establishing a specific acceptance method, the invention designs a special acceptance flow of water for mass spectrometry detection for two specific matters of metronidazole and chloramphenicol, the flow not only considers the general index of water quality, but also pays attention to the factors that may interfere with metronidazole and chloramphenicol detection, and the invention successfully reduces the interference of the water for metronidazole and chloramphenicol by optimizing the experimental conditions, selecting proper ion source and collision energy and other parameters, and the invention also establishes a corresponding accurate and blank test solution.
Finally, it should be noted that: the foregoing embodiments are merely for illustrating the technical solution of the present application, and not for limiting the same, and although the present application has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that the technical solution described in the foregoing embodiments may be modified or some or all of the technical features may be equivalently replaced, and the modification or replacement does not deviate the essence of the corresponding technical solution from the scope of the technical solution of the embodiments of the present application.
Claims (10)
1. The acceptance method of the water for detecting the metronidazole and the chloramphenicol mass spectrum is characterized by comprising the following steps of:
S1, visually observing a water sample to ensure that the water sample is colorless and transparent and has no peculiar smell so as to preliminarily judge the quality of the water sample;
s2, in a clean environment, measuring by using a high performance liquid chromatography-triple quadrupole mass spectrometer, wherein:
Selecting a water-resistant chromatographic column;
an aqueous solution for mass spectrometry containing 0.1% formic acid and a methanol solution containing 0.1% formic acid were used as mobile phase a and mobile phase B, respectively;
Preparing a reference substance stock solution by taking methanol as a solvent;
Preparing a reference substance solution and a blank solution by taking an acetonitrile solution containing 0.5% formic acid as a diluent;
S3, preparing a reference substance solution, wherein the reference substance solution comprises a mixed standard series solution of metronidazole and chloramphenicol, and the mixed standard series solution is used for determining a detection limit and drawing a standard curve;
s4, observing the peak-to-peak condition of chromatographic peaks by measuring a reference substance solution and a blank solution, and determining the detection limit of metronidazole and chloramphenicol;
S5, replacing the surface water sample as a sample solution to be measured, and if the chromatographic peak areas of the blank solution and the sample solution are smaller than the peak area corresponding to the actually measured lowest detection concentration, judging that the water sample is suitable for mass spectrum detection of metronidazole and chloramphenicol.
2. The method for checking and accepting water for detecting metronidazole and chloramphenicol according to claim 1, wherein in step S2, the measurement conditions of the high performance liquid chromatography-triple quadrupole mass spectrometer include specific liquid phase conditions and mass spectrometry conditions for precisely measuring the content of metronidazole and chloramphenicol.
3. The method for checking and accepting water for metronidazole and chloramphenicol mass spectrometry as claimed in claim 1, wherein in the step S3, the concentration is taken as an abscissa, the quantitative ion chromatographic peak area is taken as an ordinate, and the linear correlation coefficient r is more than or equal to 0.99.
4. The method for accepting water for mass spectrometry of metronidazole and chloramphenicol according to claim 1, wherein in step S3, the preparation of the mixed standard series of solutions comprises:
S31, precisely weighing 10mg of metronidazole and 10mg of chloramphenicol reference substances respectively, putting the metronidazole and the chloramphenicol reference substances into a 100mL volumetric flask, adding a solvent for dissolution and fixing the volume, and then mixing to obtain a standard stock solution with the mass concentration of 0.1 mg/mL;
s32, precisely transferring 1ml of the mixed standard stock solution into a 100ml volumetric flask, diluting with a solvent, fixing the volume to a scale, and preparing mixed standard series solutions with different concentrations by using a diluent for subsequent quantitative analysis.
5. The method for inspecting water for mass spectrometry of metronidazole and chloramphenicol according to claim 4, wherein in step S32, the standard series of solutions are mixed to obtain mixed standard series of solutions having different concentrations of S1 (2 ng/mL), S2 (5 ng/mL), S3 (20 ng/mL), S4 (60 ng/mL) and S5 (100 ng/mL) in this order.
6. The method according to claim 5, wherein in step S5, the process for determining the lowest detected concentration comprises:
S51, respectively and precisely transferring a proper amount of mixed standard working solution S1 (2 ng/mL), and diluting with a diluent until the signal to noise ratio S/N of the metronidazole and chloramphenicol peak heights reaches 3:1, namely, respectively obtaining detection limit solutions;
S52, calculating to obtain the measured lowest detected concentration based on the sampling amount of 0.2 g.
7. The method for detecting water for mass spectrometry of metronidazole and chloramphenicol as claimed in claim 6, wherein in step S52, the calculation formula of the measured minimum detected concentration includes:
；
And V is the volume of a fixed sample, the unit is milliliter, D is the dilution multiple, if not diluted, 1 is the sampling quantity, and 0.2g is taken as the sampling quantity, 2 mu L of mixed standard working solution S3 (20 ng/mL) is sampled in the subsequent measuring process, the mixed standard working solution S3 is injected into a high performance liquid chromatography-triple quadrupole mass spectrometry combined instrument, whether the peak is normal or not is observed, if the peak is normal, 2 mu L of standard series solution, detection limiting solution, blank solution and sample solution are respectively sampled, and in the process, the chromatographic peak areas of the blank solution and the sample solution are ensured to be smaller than the calculated actual measurement minimum detection concentration.
8. The method according to claim 7, wherein in step S52, the minimum detected concentration is measured to satisfy the requirement of 0.1. Mu.g/g.
9. The method for accepting water for mass spectrometry of metronidazole and chloramphenicol as claimed in claim 1, wherein the representative water sample in step S5 is ultrapure water or distilled water.
10. The method for checking and accepting water for mass spectrometry detection of metronidazole and chloramphenicol of claim 1, wherein the water sample is suitable for mass spectrometry detection of metronidazole and chloramphenicol of cosmetics such as cream, emulsion and water.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160370357A1 (en) * | 2015-06-16 | 2016-12-22 | Agilent Technologies, Inc. | Compositions and methods for analytical sample preparation |
| CN113376292A (en) * | 2021-07-09 | 2021-09-10 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Method for simultaneously determining residues of 3 veterinary drugs in honeyed pills or water-honeyed pills |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160370357A1 (en) * | 2015-06-16 | 2016-12-22 | Agilent Technologies, Inc. | Compositions and methods for analytical sample preparation |
| CN113376292A (en) * | 2021-07-09 | 2021-09-10 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Method for simultaneously determining residues of 3 veterinary drugs in honeyed pills or water-honeyed pills |
Non-Patent Citations (3)
| Title |
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| 丘福保 等: "养殖水体中 7 种甲硝唑类和 4 种氯霉素类抗生素的固相萃取-液相色谱-串联质谱测定法", 环境与健康杂志, 1 February 2024 (2024-02-01), pages 1 - 4 * |
| 中华人民共和国国家卫生和计划生育委员会 发布: "中华人民共和国国家职业卫生标准 GBZ/T 295—2017 职业人群生物监测方法 总则", 30 September 2017, pages: 1 - 12 * |
| 张海婧 等: "饮用水中甲硝唑的固相萃取-超高效液相色谱串联质谱测定法", 环境与健康杂志, vol. 33, no. 03, 31 March 2016 (2016-03-31), pages 254 - 256 * |
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