CN111537633A - Liquid chromatography-mass spectrometry combined detection method for cephalosporin antibiotics - Google Patents
Liquid chromatography-mass spectrometry combined detection method for cephalosporin antibiotics Download PDFInfo
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Abstract
The invention relates to a liquid chromatogram-mass spectrum combined detection method of cephalosporin antibiotics, which is characterized by comprising the following steps: (1) sample pretreatment: removing suspended matters from a certain amount of water sample by a centrifugal machine, then carrying out suction filtration, and then adjusting the pH value of the water sample; (2) sample extraction: leaching an extraction column for activation, adding a chelating agent into a water sample, fully mixing, passing the water sample through the extraction column, washing the extraction column after sample treatment, drying, eluting, collecting eluent, and blowing the eluent to be nearly dry to obtain residues; (3) mass spectrum detection: dissolving the residue to obtain a solution to be detected, and detecting the solution to be detected under a certain gradient elution condition and a mass spectrum detection condition. Compared with the prior art, the method has the advantages of simple operation, strong specificity, high accuracy, good tolerance, high instrument sensitivity and the like.
Description
Technical Field
The invention relates to the field of environmental analysis, in particular to a liquid chromatography-mass spectrometry combined detection method for cephalosporin antibiotics.
Background
The liquid chromatography-mass spectrometry combination is the combination of two technologies, combines high-efficiency separation and structure identification into a whole, and becomes a powerful tool for qualitative and quantitative determination of trace components in a complex mixture.
The liquid chromatography takes liquid as a mobile phase, is particularly suitable for analyzing compounds with high boiling point macromolecules, strong polarity and poor thermal stability, and is more suitable for analyzing a plurality of medicines, such as tetracyclines with thermal instability. The development of science and technology in the past decades promotes the development of a liquid mass spectrometry technology, the liquid mass spectrometry technology is a combination of a separation technology and a qualitative technology, on one hand, a liquid chromatogram has high-speed and high-efficiency separation capability and sensitivity, but only shows chromatographic peaks and retention values, cannot provide structural information of a detected component or carry out structural identification on an unknown compound, and is difficult to make qualitative judgment on the component, and on the other hand, the mass spectrum utilizes very strong structural identification capability, but does not have separation capability. The two technologies are combined to complement each other, and compounds with different properties are analyzed.
The detection of cephalosporin antibiotics in water bodies faces the following difficulties: (1) the concentration of antibiotic residues in the water body is low, and the majority of the antibiotic residues are in the magnitude of mu g/L or ng/L; (2) more than one antibiotic is left in the water body, and a plurality of methods for detecting simultaneously need to be developed, so that the sampling amount is reduced and the time is saved; (3) impurities in the water can interfere with the detection of antibiotics, reducing the sensitivity of the method. With the increasingly hybridization of practical water samples and the increase of the types of cephalosporin antibiotics in the water samples, a method which has a lower method quantification limit and can simultaneously detect more cephalosporin antibiotics at a time is required in recent years.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a liquid chromatography-mass spectrometry combined detection method for cephalosporin antibiotics, which solves the problems that the cephalosporin antibiotics in water are low in concentration and many in impurities, and can not be used for simultaneously measuring multiple antibiotics.
The purpose of the invention can be realized by the following technical scheme:
a detection method for liquid chromatography-mass spectrometry combination of cephalosporin antibiotics comprises the following steps:
(1) sample pretreatment: removing suspended matters from a certain amount of water sample by a centrifugal machine, then carrying out suction filtration, and then adjusting the pH value of the water sample;
(2) sample extraction: leaching an extraction column for activation, adding a chelating agent into a water sample, fully mixing, passing the water sample through the extraction column, washing the extraction column after sample treatment, drying, eluting, collecting eluent, and blowing the eluent to be nearly dry to obtain residues;
(3) mass spectrum detection: dissolving the residue to obtain a solution to be detected, and detecting the solution to be detected under a certain gradient elution condition and a mass spectrum detection condition.
Further, the rotation speed of the centrifuge in the step (1) is 4000-; the suction filtration adopts a glass fiber filter membrane with the aperture of 0.2-0.5 mu m; the pH value of the water sample is adjusted by 0.5M hydrochloric acid, and the pH value is adjusted to be 1.5-5.5, preferably 2.5-4.5, and more preferably 2.5.
Further, the activation in the step (2) is carried out by leaching the extraction column with methanol and ultrapure water which are equal in volume; the chelating agent comprises Na2EDTA, the volume ratio of the water sample to the chelating agent is (40-60) to 1; the water sample is passed through the extraction column at a flow rate of 2-10 ml/min.
Further, the rinsing in the step (2) is rinsing with ultrapure water, and the drying is performed for 10-30min under the protection of nitrogen; the eluent is a mixed liquid of methanol and water in a volume ratio of (60-100) to (0-40), the dosage of the eluent is 0.4-1.2% of the volume of the water sample, and the step of blowing to near dryness is that blowing to near dryness under the protection of nitrogen.
Further, the dissolution residue in the step (3) is dissolved by using the water sample volume 1/1000 of methanol.
Further, the gradient elution conditions in step (3) are as follows:
mobile phase: a is 0.1 percent of formic acid solution by volume ratio, B is methanol;
gradient elution conditions: 0-1.0min, 5% B; 1.0-4.5min, 5-50% B; 4.5-7.5min, 50-70% B; 7.5-7.6min, 70-5% B; 7.6-9min, 0.5% B; the flow rate was 0.30ml/min, and the amount of sample was 10. mu.L, as shown in Table 1:
TABLE 1 gradient elution procedure
Further, the mass spectrum detection conditions in the step (3) are as follows:
the ion source is an ESI source, the capillary voltage is 2.0-4.0kV, the extraction taper hole voltage is 20-30V, the RF lens voltage is 0.2-0.8V, the ion source temperature is 125--1The air flow rate of the taper hole is 30-60L/h.
Further, the extraction column used was a 6cc/200mg extraction column from Waters corporation.
Further, the chromatographic column adopts an Acquity BEH C18 chromatographic column.
Further, the cephalosporin antibiotics comprise one or more of cefaclor, ceftriaxone, ceftazidime, ceftiofur or cephalexin.
Compared with the prior art, the invention has the beneficial effects that:
(1) a plurality of cephalosporin antibiotics target objects can be simultaneously measured;
(2) the centrifuge is adopted for pretreatment and the extraction column is used for concentration, the pretreatment step is simple, other interferents can be effectively removed, and the specificity is good;
(3) the detection is carried out by adopting a liquid chromatography-mass spectrometry combined technology, the detection time is short, and the sensitivity is high.
(4) The optimal concentration is selected by comparing the concentrations of the elution solvent in different proportions, so that the recovery rate of the substance to be detected is improved.
(5) The optimal pH value is adjusted through a contrast test, so that the experimental recovery rate is obviously improved.
Drawings
FIG. 1 is a schematic diagram showing the peak appearance of the detection method of liquid chromatography-mass spectrometry in example 1;
FIG. 2 is a standard curve diagram showing a detection method of liquid chromatography-mass spectrometry in example 1;
FIG. 3 is a comparison of the liquid chromatography-mass spectrometry detection method of the present invention versus the ratio of eluting solvent;
FIG. 4 is a graph comparing pH with a liquid chromatography-mass spectrometry detection method according to the present invention;
FIG. 5 is a graph showing a comparison of the amount of elution solvent in the detection method of the present invention using a combination of liquid chromatography and mass spectrometry.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
A liquid chromatography-mass spectrometry combined detection method for cephalosporin antibiotics in sewage comprises the following steps: an analysis method for detecting cephalosporin antibiotics by liquid chromatography-mass spectrometry is used for analyzing and researching cephalosporin antibiotic spectrograms in water samples in different areas, establishing a liquid chromatography-mass spectrometry combined comparison spectrogram and providing a basis for monitoring and evaluating cephalosporin antibiotic wastewater.
The reagents and instruments used in the examples below and the laboratory kits are commercially available. The reagents and instruments used were as follows:
1. reagent
Cefuroxime, cephalexin, cephradine, ceftazidime, ceftiofur, cefaclor and cefotaxime are all available from Tianjin Azta technologies, Inc.; ethylenediaminetetraacetic acid disodium salt (Na)2EDTA), methanol, formic acid and hydrochloric acid (available from j.t. baker).
2. Instrument for measuring the position of a moving object
TQD ultra high liquid chromatography triple quadrupole mass spectrometer (Waters, USA); a centrifugal machine (Xiang appearance TGL-16M); vacuum pump (SCICHRO, model SCI-NV 40B); a 24-tube solid phase extraction unit (SCICHRO, model DC 150-2); nitrogen blowing instrument (hang zhou youning instruments ltd, model DC 150-2); vortex mixer (Kylin-bell, model QL-902); a pH meter (Raymond magnetic DHS-25); a sand core filtration device (Tianjingtiang test equipment ltd); oasis HLB solid phase extraction column 6cc/200mg (Waters corporation); chromatography Column (ACQUITY UPLC BEH C18 Column,1.7 μm,2.1 mm. times.50 mm, 1/pkg); glass fiber filters (Collins water system filters-polyethersulfone membranes).
The mass spectrum parameters of the target analytes for quantitative analysis are shown in table 2, and the correlation coefficient and the lower limit of quantitation of each analyte are shown in table 3.
Table 2 mass spectrometry parameters of target analytes for quantitative analysis
3. Sensitivity and linear range
And (3) precisely weighing cefalexin, cefradine, cefaclor, cefuroxime and cefotaxime reference substances by using an analytical balance, dissolving the reference substances by using methanol, diluting into standard solutions with a series of concentrations, and detecting according to the conditions. And (4) performing regression by taking the concentration as an abscissa and the response value as an ordinate to obtain a standard curve. The standard curve range, correlation coefficient and lower limit of quantification of each object to be measured are shown in Table 3
TABLE 3 correlation coefficient and lower limit of quantitation for each analyte
Example 1
1. Preparation of a standard solution:
10mg of each standard sample was weighed, placed in a beaker, and dissolved in 100ml of methanol to prepare a 10mg/L standard solution, which was stored at-20 ℃. Mixing standards with different concentrations are prepared according to the required concentration.
2. Sample pretreatment
Taking 1L of water sample containing cefalexin, cefradine, cefaclor, cefuroxime and cefotaxime in a sewage treatment plant, and removing suspended matters by a centrifugal machineAnd after centrifugation, the water sample is filtered by a 0.222 mu m glass fiber filter membrane. The pH of the water sample was adjusted to 2.5 by the addition of 0.5M HCl. 20ml of Na was added2EDTA and mixed well. And (3) extracting the water sample through an HLB (hydrophile-lipophile balance) extraction column. The column was first rinsed with 10ml methanol and 10ml ultrapure water for activation. The water sample was passed through the extraction column at a flow rate of 5 ml/min. The post-sample column was washed with 10ml of ultra pure water and dried under nitrogen for 20 min. Then eluting with 12ml methanol twice, collecting eluent, blowing nitrogen to near dryness, and fixing volume with 1ml methanol to be tested.
3. Conditions of the apparatus
A chromatographic column: acquity BEH C18(100 mm. times.2.1 mm,1.7 μm);
mobile phase A: 0.1% formic acid solution, mobile phase B: methanol;
gradient elution conditions: 0-1.0min, 5% B; 1.0-4.5min, 5-50% B; 4.5-7.5min, 50-70% B; 7.5-7.6min, 70-5% B; 7.6-9min, 0.5% B; the flow rate is 0.30 ml/min; the amount of the sample was 10. mu.L.
Mass spectrum conditions: the ion source is an ESI source, the capillary voltage is 2.0-4.0kV, the extraction taper hole voltage is 20-30V, the RF lens voltage is 0.2-0.8V, the ion source temperature is 125--1The air flow rate of the taper hole is 30-60L/h.
Example 2
Except for the difference from example 1, the pH of the water sample was adjusted to 1.5 by adding 0.5M HCl.
Example 3
Except for the difference from example 1, the pH of the water sample was adjusted to 3.5 by adding 0.5M HCl.
Example 4
Except for the difference from example 1, the pH of the water sample was adjusted to 4.5 by adding 0.5M HCl.
Example 5
Except for the difference from example 1, the pH of the water sample was adjusted to 5.5 by adding 0.5M HCl.
Table 5 shows the relationship between pH and the recovery rate of the target analyte in examples 1 to 5, and it can be seen that the recovery rates of the respective substances were good in the range of pH 1.5 to 5.5, and particularly, the recovery rate of the antibiotic was extremely excellent in the range of 84.03 to 94.56% at pH 2.5, as shown in fig. 3.
TABLE 5 recovery and relative standard deviation of target analytes at different pH
Example 6
The difference from example 1 is that elution was carried out in two portions using 12ml of a mixed liquid of methanol and water at a volume ratio of 90: 10.
Example 7
The difference from example 1 is that elution was carried out in two portions using 12ml of a mixed liquid of methanol and water at a volume ratio of 80: 20.
Example 8
The difference from example 1 is that elution was carried out in two portions using 12ml of a mixed liquid of methanol and water at a volume ratio of 70: 30.
Example 9
The difference from example 1 is that elution was carried out in two portions using 12ml of a mixed liquid of methanol and water at a volume ratio of 60: 40.
As shown in fig. 4, examples 1 and 6 to 9 showed good recovery under the test conditions, especially, the recovery of each substance was 80% or more by elution with 100% methanol.
Example 10
The difference from example 1 is that elution was carried out twice with 4ml of methanol.
Example 11
The difference from example 1 is that elution was carried out twice with 6ml of methanol.
Example 12
The difference from example 1 is that elution was carried out twice with 8ml of methanol.
Example 13
The difference from example 1 is that elution was carried out twice with 10ml of methanol.
As shown in FIG. 5, examples 1 and 10 to 13 showed good recovery under the test conditions, especially, the recovery of each substance was 80% or more by elution with 12ml of methanol.
In the description herein, references to the description of the terms "embodiment," "example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Claims (10)
1. A detection method for liquid chromatography-mass spectrometry combination of cephalosporin antibiotics is characterized by comprising the following steps:
(1) sample pretreatment: removing suspended matters from a certain amount of water sample by a centrifugal machine, then carrying out suction filtration, and then adjusting the pH value of the water sample;
(2) sample extraction: leaching an extraction column for activation, adding a chelating agent into a water sample, fully mixing, passing the water sample through the extraction column, washing the extraction column after sample treatment, drying, eluting, collecting eluent, and blowing the eluent to be nearly dry to obtain residues;
(3) mass spectrum detection: dissolving the residue to obtain a solution to be detected, and detecting the solution to be detected under a certain gradient elution condition and a mass spectrum detection condition.
2. The method for detecting the combination of liquid chromatography and mass spectrometry of cephalosporin antibiotics as claimed in claim 1, characterized in that the rotation speed of the centrifuge in step (1) is 4000-; the suction filtration adopts a glass fiber filter membrane with the aperture of 0.2-0.5 mu m; the pH value of the water sample is adjusted by 0.5M hydrochloric acid, and the pH value is adjusted to be 1.5-5.5.
3. The method for detecting cephalosporin antibiotics in combination of liquid chromatography-mass spectrometry as claimed in claim 1, characterized in that the activation in step (2) is carried out by rinsing the extraction column with methanol and ultrapure water of equal volume; the above-mentionedThe chelating agent comprises Na2EDTA, the volume ratio of the water sample to the chelating agent is (40-60) to 1; the water sample is passed through the extraction column at a flow rate of 2-10 ml/min.
4. The method for detecting cephalosporin antibiotics in combination of liquid chromatography-mass spectrometry as claimed in claim 1, characterized in that, the rinsing in step (2) is rinsing with ultrapure water, and the drying is drying for 10-30min under nitrogen protection; the eluent is a mixed liquid of methanol and water in a volume ratio of (60-100) to (0-40), the dosage of the eluent is 0.4-1.2% of the volume of the water sample, and the step of blowing to near dryness is that blowing to near dryness under the protection of nitrogen.
5. The method for detecting cephalosporin antibiotics in combination of liquid chromatography-mass spectrometry as claimed in claim 1, wherein the dissolution residue in step (3) is dissolved with 1/1000 sample volume of methanol.
6. The method for detecting cephalosporin antibiotics in combination of liquid chromatography-mass spectrometry as claimed in claim 1, characterized in that, the gradient elution conditions in step (3) are as follows:
mobile phase: a is 0.1 percent of formic acid solution by volume ratio, B is methanol;
gradient elution conditions: 0-1.0min, 5% B; 1.0-4.5min, 5-50% B; 4.5-7.5min, 50-70% B; 7.5-7.6min, 70-5% B; 7.6-9min, 0.5% B; the flow rate was 0.30ml/min and the amount of sample was 10. mu.L.
7. The method for detecting cephalosporin antibiotics in combination of liquid chromatography-mass spectrometry as claimed in claim 1, characterized in that the mass spectrometry detection conditions in step (3) are as follows:
the ion source is an ESI source, the capillary voltage is 2.0-4.0kV, the extraction taper hole voltage is 20-30V, the RF lens voltage is 0.2-0.8V, the ion source temperature is 125--1The air flow rate of the taper hole is 30-60L/h.
8. The method for detecting cephalosporin antibiotics in combination of liquid chromatography-mass spectrometry as claimed in claim 1, characterized in that the extraction column is a Waters 6cc/200mg extraction column.
9. The method for detecting cephalosporin antibiotics in combination of liquid chromatography-mass spectrometry as claimed in claim 1, characterized in that the chromatographic column adopts an Acquity BEH C18 chromatographic column.
10. The method for detecting cephalosporin antibiotics of claim 1, wherein the cephalosporin antibiotics comprise one or more of cefaclor, ceftazidime, ceftiofur or cephalexin.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113376295A (en) * | 2021-05-24 | 2021-09-10 | 安徽万邦医药科技股份有限公司 | Method for measuring concentration of cefradine in human blood plasma |
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2020
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| WO2008117079A1 (en) * | 2007-03-28 | 2008-10-02 | Helperby Therapeutics Limited | Antimicrobial compounds based upon 4-aminoquinoline |
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| CN113376295A (en) * | 2021-05-24 | 2021-09-10 | 安徽万邦医药科技股份有限公司 | Method for measuring concentration of cefradine in human blood plasma |
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Application publication date: 20200814 |