CN114113371A - Liquid chromatography-mass spectrometry detection method for cephalosporin C in cephalosporin residues - Google Patents
Liquid chromatography-mass spectrometry detection method for cephalosporin C in cephalosporin residues Download PDFInfo
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Abstract
The invention discloses a method for detecting cephalosporin C in cephalosporin slag, which comprises the following steps: a. preparing a standard solution; b. preparing a test solution; c. respectively sucking standard curve working solution and sample solution, and injecting into an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer; the chromatographic conditions are as follows: a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; mobile phase: methanol and 0.1% formic acid in a volume ratio of 10: 90; the mass spectrum conditions are as follows: an ionization mode: electrospray positive ions; scanning mode: multiple Reaction Monitoring (MRM). The invention has simple and quick operation and low cost; the method has the advantages of high accuracy and sensitivity, strong specificity and good reproducibility, and can quickly and effectively detect the residual quantity of cephalosporin C in the cephalosporin dregs.
Description
Technical Field
The invention relates to the technical field of detection, and particularly relates to a liquid chromatography-mass spectrometry detection method for cephalosporin C in cephalosporin residues.
Background
Cephalosporin C is mainly used as an intermediate for preparing 7-aminocephalosporanic acid (7-ACA), and is one of antibiotics produced by penicillium closely related cephalosporium fungi. The residual culture medium residue after the fungus fermentation production, hereinafter referred to as "mushroom residue", contains rich nutrient substances, wherein the content of protein and polysaccharide is high, so that the transformation of the mushroom residue into fertilizer and feed is an economic and effective choice for many pharmaceutical factories, but meanwhile, the mushroom residue contains a large amount of mycelium, and if the mushroom residue is not properly treated, secondary fermentation can be caused, peculiar smell is generated, water body is polluted, and potential risk of generating drug resistance genes can be caused. In the national records of hazardous waste revised in 2008, the antibiotic residues are listed as a hazardous waste, so the harmless treatment and resource utilization of the antibiotic residues become important difficult problems to be solved urgently in the whole industry.
At present, no standard detection method for cephalosporin C residues in cephalosporin residues exists at home and abroad, the pretreatment steps reported by the existing data are very complicated, repeated organic reagent extraction is needed, or a solid phase extraction device is used for purification, so that the sample pretreatment cost is increased, a high performance liquid chromatograph is usually adopted and an ultraviolet detector is configured for detection, but the molar absorption coefficient of the cephalosporin C is not high enough, so that the detection method cannot meet the requirement of quickly detecting the low content of the cephalosporin C in the cephalosporin residues.
Disclosure of Invention
In order to solve the problems, the invention provides a method for detecting cephalosporin C in cephalosporin residues, which comprises the following steps:
a. preparation of a standard solution: adding water into a cephalosporin C standard substance to prepare a standard substance solution;
b. preparing a test solution: taking a sample to be tested, adding water, mixing uniformly, carrying out vortex and centrifugation, taking supernate, and filtering to obtain a test sample solution;
c. respectively sucking the standard solution and the test solution, and injecting into an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer;
the chromatographic conditions are as follows: a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; mobile phase: methanol and 0.1% formic acid in a volume ratio of 10: 90;
the mass spectrum conditions are as follows: an ionization mode: electrospray positive ions; scanning mode: multiple Reaction Monitoring (MRM).
Further, the mass volume ratio of the sample to be detected in the step b to water is 0.5-1.5 g:10ml, preferably 1g:10 ml; and/or the water of step a) and step b) is deionized water.
Further, the preparation process of the standard solution in the step a is carried out in an ice box, and the prepared standard solution is detected in time or placed in a refrigerator at 4 ℃ to be detected; and c, the preparation process of the test solution in the step b is carried out in an ice box, and the prepared test solution is detected in time or placed in a refrigerator at 4 ℃ to be detected.
Further, after uniformly mixing, performing vortex oscillation for 3-10 min, preferably for 5 min; the centrifugal speed is 2000-5000 rpm/min, the time is 5-20 min, the preferred speed is 4000rpm/min, and the time is 10 min; the filtration is carried out by using a 0.22 mu m inorganic microporous filter membrane.
Further, the chromatographic column of the chromatographic conditions of the step C) is a Waters-C18 column with the specification of 2.1X 50mm and 1.7 μm; the sample amount is 1-25 μ L, preferably 10 μ L; the column temperature is 20-45 DEG CPreferably 35 ℃; the flow rate is 0.1-0.3 mL/min-1Preferably 0.25mL/min-1。
Further, the ion source temperature of the mass spectrum condition of step c) is 150 ℃; the temperature of the desolvation gas is 450 ℃; the flow rate of the desolventizing agent is 650L/h; the spraying voltage is 3.2 kv; the voltage of the taper hole is 24V; the collision voltage is 18V; the parent ion m/z was scanned at 416.09, the quantifier ion m/z was 142.99, and the quantifier ion m/z was 184.99.
The invention also provides a method for measuring the content of cephalosporin C in cephalosporin slag, which comprises the following steps:
1) preparation of standard curve working solution of series concentration
Respectively taking the same amount of cephalosporin C residue-free cephalosporin residues, adding the standard solution and water in the step a, uniformly mixing, vortexing, centrifuging, taking supernatant, and filtering to prepare a series of standard curve working solutions with concentration;
2) and (3) determining the content of cephalosporin C in the sample to be detected:
and (C) respectively taking a standard curve working solution with a series of concentrations and the test solution in the step b, injecting the standard curve working solution and the test solution in the step b into an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer, detecting according to the conditions in the step C, drawing a standard curve according to the concentration of the standard working solution and the measured peak area, and obtaining the content of cephalosporin C in the sample to be detected according to the standard curve.
Further, the concentration of the cephalosporin C in the standard curve working solution in the step 1) is 1.0-500.0 mu g/L.
Further, the concentrations of cephalosporin C in the working solution of the standard curve are 1.0. mu.g/L, 5.0. mu.g/L, 25.0. mu.g/L, 100.0. mu.g/L and 500.0. mu.g/L.
Still further, the standard curve working solution was placed in a 4 ℃ refrigerator.
Further, carrying out vortex oscillation for 3-10 min, preferably for 5min in the step 1); the centrifugal speed is 2000-5000 rpm/min, the time is 5-20 min, the preferred speed is 4000rpm/min, and the time is 10 min; the filtration is carried out by using a 0.22 mu m inorganic microporous filter membrane.
The invention provides an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer detection method for cephalosporin C in cephalosporin residues, wherein the qualitative detection limit of the method is 10.0 mug/kg, and the quantitative limit of the method is 35.0 mug/kg; when the standard concentration level of the sample is 400ng/g, the recovery rate is 100.7-109.6%; compared with the prior art, the method can avoid the decomposition of the cephalosporin C as much as possible, and improve the accuracy of the detection method; complex processes such as solid phase extraction or repeated solvent extraction are not needed, the operation is simple and rapid, and the cost is low; the method has the advantages of high accuracy and sensitivity, strong specificity and good reproducibility, and can quickly and effectively detect the residual quantity of cephalosporin C in the cephalosporin dregs.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 is a process flow diagram;
FIG. 2 is a total ion flow diagram of a cephalosporin C residue-free cephalosporin C sample in example 1;
FIG. 3 is a total ion flow diagram of a cephalosporin C residue-free cephalosporin C residue-labeled sample in example 1.
The specific implementation mode is as follows:
example 1 detection of cephalosporin C in cephalosporin residue according to the invention
1) Preparation of Standard solutions
a. Preparation of a standard solution: taking a cephalosporin C standard substance, and adding deionized water to prepare a cephalosporin C standard substance solution;
b. preparing a test solution: preparing a sample to be tested: accurately weighing 1.0g of a cephalosporin residue sample in a colorimetric tube, adding a deionized water solution, shaking up, fixing the volume to 10ml, carrying out vortex oscillation for 5min, then centrifuging at 4000rpm/min for 10min, taking supernatant, passing the supernatant through a 0.22-micron inorganic microporous filter membrane to obtain a sample, and placing the sample in an ice bath to be detected;
c. respectively sucking the standard solution and the test solution, and injecting into an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer;
chromatographic conditions are as follows: the column was a Waters-C18 column (2.1 × 50mm, 1.7 μm) with methanol: 0.1% formic acid: 10:90 as mobile phase; the flow rate is 0.25 mL/min; the column temperature was 35 ℃ and the amount of sample was 10. mu.L.
Mass spectrum conditions: the ionization mode is an electrospray positive ion mode; the ion source temperature is 150 ℃; the temperature of the desolvation gas is 450 ℃; the flow rate of the desolventizing agent is 650L/h; the spraying voltage is 3.2 kv; the voltage of the taper hole is 24V; the collision voltage is 18V; the scan mode was a Multiple Reaction Monitoring (MRM) mode, the parent ion m/z was scanned at 416.09, the daughter ion m/z was scanned at 142.99, and the daughter ion m/z was scanned at 184.99.
And (3) displaying a corresponding chromatographic peak and retention time of the cephalosporin C in the standard substance spectrum in the test sample spectrum, namely residual cephalosporin C in the cephalosporin residue.
Example 2 detection of sulfate ions in the motherwort injection of the present invention
The instrument comprises the following steps: ultra performance liquid chromatography-triple quadrupole tandem mass spectrometer.
Chromatographic conditions are as follows: the column was a Waters-C18 column (2.1 × 50mm, 1.7 μm) with methanol: 0.1% formic acid: 10:90 as mobile phase; the flow rate is 0.25 mL/min; the column temperature was 35 ℃ and the amount of sample was 10. mu.L.
Mass spectrum conditions: the ionization mode is an electrospray positive ion mode; the ion source temperature is 150 ℃; the temperature of the desolvation gas is 450 ℃; the flow rate of the desolventizing agent is 650L/h; the spraying voltage is 3.2 kv; the voltage of the taper hole is 24V; the collision voltage is 18V; the scan mode was a Multiple Reaction Monitoring (MRM) mode, the parent ion m/z was scanned at 416.09, the daughter ion m/z was scanned at 142.99, and the daughter ion m/z was scanned at 184.99.
1) Preparing a sample to be tested: accurately weighing 1.0g of a cephalosporin residue sample in a colorimetric tube, adding a deionized water solution, shaking up, fixing the volume to 10ml, carrying out vortex oscillation for 5min, then centrifuging at 4000rpm/min for 10min, taking supernatant, passing the supernatant through a 0.22-micron inorganic microporous filter membrane to obtain a sample, and placing the sample in an ice bath to be detected.
2) Drawing a standard curve: accurately weighing 5 parts of a bacterial residue sample without cephalosporin C residue in a colorimetric tube, sequentially adding a certain amount of cephalosporin C standard solution described in embodiment 1, adding deionized water, shaking up and fixing the volume to 10ml to obtain standard working solutions with cephalosporin C concentrations of 1.0 μ g/L, 5.0 μ g/L, 25.0 μ g/L, 100.0 μ g/L and 500.0 μ g/L, carrying out vortex oscillation for 5min, centrifuging at 4000rpm/min for 10min, taking supernatant, passing the supernatant through a 0.22 μm inorganic microporous filter membrane to obtain a standard working solution, placing the standard working solution in an ice bath, carrying out detection and analysis by adopting an ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometer, drawing a standard curve by measuring peak area and corresponding standard working solution concentration, and calculating a regression equation and a correlation coefficient.
3) Detection and analysis: and (3) injecting the standard working solution and the test solution into an ultra-high performance liquid chromatograph, detecting by adopting the chromatographic and mass spectrum conditions described in the embodiment 1, and calculating the residual quantity of the cephalosporin C according to an external standard method.
The advantageous effects of the present invention are explained below by way of test examples
Test example 1 methodological verification of the invention
1. Method of producing a composite material
1) Preparation of the respective solutions
a. Preparation of a standard solution: taking a cephalosporin C standard substance, adding deionized water to prepare a cephalosporin C standard substance solution with the concentration of 1000mg/L, diluting the solution step by step into cephalosporin C series concentration standard substance solutions with the concentrations of 5 mug/L, 10 mug/L, 20 mug/L, 35 mug/L, 50 mug/L, 250 mug/L, 400 mug/L, 1250 mug/L, 5000 mug/L and 25000 mug/L respectively, wherein the operation needs to be carried out on an ice box, and the prepared intermediate standard substance solution is placed on the ice box for standby;
b. preparation of standard curve working solution: accurately weighing 5 parts of 1.0g of a bacteria residue sample without cephalosporin C residue in a 25ml colorimetric tube, then respectively adding 200 mul of cephalosporin C intermediate standard solution with the concentration of 50 mug/L, 250 mug/L, 1250 mug/L, 5000 mug/L and 25000 mug/L, then adding deionized water, shaking up and fixing the volume to 10ml, carrying out vortex oscillation for 5min, then centrifuging at 4000rpm/min for 10min, taking the supernatant, putting the supernatant into a liquid phase vial after passing through a 0.22 mu m inorganic microporous filter membrane to prepare cephalosporin C standard curve working solutions with the concentrations of 1.0 mug/L, 5.0 mug/L, 25.0 mug/L, 100.0 mug/L and 500.0 mug/L respectively, and detecting or placing in a refrigerator at 4 ℃ in time for detection;
c. sample test solution preparation: accurately weighing 6 parts of 1.0g of cephalosporin residue sample in a 25ml colorimetric tube;
d. preparation of recovery rate test solution: accurately weighing 2 parts of 1.0g of a bacterial residue sample without cephalosporin C residue in a 25ml colorimetric tube, and respectively adding 1ml of a cephalosporin C intermediate standard solution with the concentration of 400 mug/L;
e. preparing a test solution with detection limit and quantification limit: accurately weighing 5 parts of 1.0g of the bacterial residue sample without cephalosporin C residue in a 25ml colorimetric tube, and respectively adding 1ml of cephalosporin C intermediate standard solution with the concentration of 5 mug/L, 10 mug/L, 20 mug/L, 35 mug/L and 50 mug/L.
2) And (3) adding deionized water into the colorimetric tubes of c, d and e, shaking up, fixing the volume to 10ml, carrying out vortex oscillation for 5min, centrifuging for 10min at 4000rpm/min, taking supernatant, filtering the supernatant through an inorganic microporous filter membrane of 0.22 mu m, filling the supernatant into a liquid phase small bottle to prepare corresponding solution (the solution prepared in each operation step is detected in time or is placed in a refrigerator at 4 ℃ to be detected), and sequentially injecting the solution into an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer for detection and analysis after all the solutions are prepared.
3) The instrument conditions were as follows:
chromatographic conditions are as follows: the chromatographic column was a Waters-C18 column (a method for determining cephalosporin C in cephalosporin residue 2.1 × 50mm, 1.7 μm), and the mobile phase was methanol: 0.1% formic acid: 10: 90; the flow rate is 0.25 mL/min; the column temperature was 35 ℃ and the amount of sample was 10. mu.L.
Mass spectrum conditions: the ionization mode is an electrospray positive ion mode; the ion source temperature is 150 ℃; the temperature of the desolvation gas is 450 ℃; the flow rate of the desolventizing agent is 650L/h; the spraying voltage is 3.2 kv; the voltage of the taper hole is 24V; the collision voltage is 18V; the scan mode was a Multiple Reaction Monitoring (MRM) mode, the parent ion m/z was scanned at 416.09, the daughter ion m/z was scanned at 142.99, and the daughter ion m/z was scanned at 184.99.
And (3) displaying a corresponding chromatographic peak and retention time of the cephalosporin C in the standard substance spectrum in the test sample spectrum, namely residual cephalosporin C in the cephalosporin residue.
4) Results of the experiment
The results of examining the various indices are shown in Table 1.
TABLE 1 validation index
As can be seen from table 1: drawing a standard curve by using the peak area of the measured working solution of the standard curve and the corresponding concentration, solving a regression equation and a correlation coefficient, and showing that the linear relation of the peak area of the cephalosporin C is good from the result (R)2Not lower than 0.9991).
Substituting the peak areas of the C and d test solution into a regression equation to calculate the concentration of cephalosporin C in each test solution; and then according to the concentration of the cephalosporin C in 6 parts of the test solution in C, the RSD is 4.1 percent, which shows that the method has good repeatability; according to the concentration of the cephalosporin C in the test solution, the recovery rate is 100.7-109.6%, which shows that the method has good accuracy;
c. calculating the ratio (namely the signal-to-noise ratio) of the response value of the chromatographic peak in the test solution with each concentration of e to the noise nearest to the chromatographic peak of cephalosporin C to obtain that the detection limit of the method is 10.0 mu g/kg (about 3 times the signal-to-noise ratio); the limit of quantitation was 35.0. mu.g/kg (about 10 times the signal-to-noise ratio), indicating a high sensitivity of the method.
In conclusion, the liquid chromatography-mass spectrometry detection method for cephalosporin C in cephalosporin residues has the advantages of high accuracy, high sensitivity and good reproducibility, can quickly and effectively detect the residual quantity of cephalosporin C in cephalosporin residues, and has good application prospects in harmless treatment and resource utilization of cephalosporin residues.
Claims (11)
1. A method for detecting cephalosporin C in cephalosporin dregs is characterized in that: it comprises the following steps:
a. preparation of a standard solution: adding water into the cephalosporin C standard to prepare a standard solution;
b. preparing a test solution: taking a sample to be tested, adding water, mixing uniformly, carrying out vortex and centrifugation, taking supernate, and filtering to obtain a test sample solution;
c. respectively sucking the standard solution and the test solution, and injecting into an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer;
the chromatographic conditions are as follows: a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; mobile phase: methanol and 0.1% formic acid in a volume ratio of 10: 90;
the mass spectrum conditions are as follows: an ionization mode: electrospray positive ions; scanning mode: multiple Reaction Monitoring (MRM).
2. The detection method according to claim 1, characterized in that: the mass volume ratio of the sample to be detected to water in the step b is 0.5-1.5 g:10ml, preferably 1g:10 ml; and/or, the water in the step a) and the step b) is deionized water.
3. The detection method according to claim 1, characterized in that: the preparation process of the standard solution in the step a is carried out in an ice box, and the prepared standard solution is detected in time or placed in a refrigerator at 4 ℃ to be detected; and c, the preparation process of the test solution in the step b is carried out in an ice box, and the prepared test solution is detected in time or placed in a refrigerator at 4 ℃ to be detected.
4. The detection method according to claim 1, characterized in that: after uniformly mixing, performing vortex oscillation for 3-10 min, preferably for 5 min; the centrifugal speed is 2000-5000 rpm/min, the time is 5-20 min, the preferred speed is 4000rpm/min, and the time is 10 min; the filtration is carried out by using a 0.22 mu m inorganic microporous filter membrane.
5. The detection method according to claim 1, characterized in that: the chromatographic column under the chromatographic condition of the step C) is a Waters-C18 column with the specification of 2.1 multiplied by 50mm and 1.7 mu m; the sample amount is 1-25 μ L, preferably 10 μ L; the column temperature is 20-45 ℃, preferably 35 ℃; the flow rate is 0.1-0.3 mL/min-1Preferably 0.25mL/min-1。
6. The detection method according to claim 1, characterized in that: step c) the ion source temperature of the mass spectrometry conditions is 150 ℃; the temperature of the desolvation gas is 450 ℃; the flow rate of the desolventizing agent is 650L/h; the spraying voltage is 3.2 kv; the voltage of the taper hole is 24V; the collision voltage is 18V; the parent ion m/z was scanned at 416.09, the quantifier ion m/z was 142.99, and the quantifier ion m/z was 184.99.
7. A method for measuring the content of cephalosporin C in cephalosporin slag is characterized in that: it comprises the following steps:
1) preparation of standard curve working solution of series concentration
Respectively taking the same amount of cephalosporin C residue-free cephalosporin residues, adding the standard solution and water in the step a, uniformly mixing, vortexing, centrifuging, taking supernatant, and filtering to prepare a series of standard curve working solutions with concentration;
2) determination of cephalosporin C content in sample to be tested
And (C) respectively taking a standard curve working solution with a series of concentrations and the test solution in the step b, injecting the standard curve working solution and the test solution in the step b into an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer, detecting according to the conditions in the step C, drawing a standard curve according to the concentration of the standard working solution and the measured peak area, and obtaining the content of cephalosporin C in the sample to be detected according to the standard curve.
8. The content measurement method according to claim 7, characterized in that: the concentration of cephalosporin C in the working solution of the standard curve in the step 1) is 1.0-500.0 mug/L.
9. The content measurement method according to claim 8, characterized in that: the concentrations of cephalosporin C in the standard curve working solution are 1.0 mug/L, 5.0 mug/L, 25.0 mug/L, 100.0 mug/L and 500.0 mug/L.
10. The content measurement method according to claim 8 or 9, characterized in that: the standard curve working solution was placed in a 4 ℃ refrigerator.
11. The content measurement method according to claim 7, characterized in that: step 1), carrying out vortex oscillation for 3-10 min, preferably for 5 min; the centrifugal speed is 2000-5000 rpm/min, the time is 5-20 min, the preferred speed is 4000rpm/min, and the time is 10 min; the filtration is carried out by using a 0.22 mu m inorganic microporous filter membrane.
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| US4577013A (en) * | 1983-12-22 | 1986-03-18 | Ciba-Geigy Corporation | Ionically modified cellulose material, its preparation and its use |
| CN108267521A (en) * | 2017-12-28 | 2018-07-10 | 伊犁川宁生物技术有限公司 | The assay method of cephalosporin residual potency in a kind of cephalo bacteria residue |
| CN110763786A (en) * | 2019-11-15 | 2020-02-07 | 中国农业科学院农业质量标准与检测技术研究所 | Method for identifying cephalosporin dregs in plant-derived protein feed raw materials and application |
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- 2021-11-03 CN CN202111294387.2A patent/CN114113371A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4577013A (en) * | 1983-12-22 | 1986-03-18 | Ciba-Geigy Corporation | Ionically modified cellulose material, its preparation and its use |
| CN108267521A (en) * | 2017-12-28 | 2018-07-10 | 伊犁川宁生物技术有限公司 | The assay method of cephalosporin residual potency in a kind of cephalo bacteria residue |
| CN110763786A (en) * | 2019-11-15 | 2020-02-07 | 中国农业科学院农业质量标准与检测技术研究所 | Method for identifying cephalosporin dregs in plant-derived protein feed raw materials and application |
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| Title |
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| 常艳等: "经不同无害化及资源化技术处理后头孢菌素C发酵菌渣中抗菌活性物质的变化情况", 《常艳》 * |
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