CN113325109A - Method for detecting residual quantity of lincomycin in mushroom dregs - Google Patents

Method for detecting residual quantity of lincomycin in mushroom dregs Download PDF

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Publication number
CN113325109A
CN113325109A CN202110629137.3A CN202110629137A CN113325109A CN 113325109 A CN113325109 A CN 113325109A CN 202110629137 A CN202110629137 A CN 202110629137A CN 113325109 A CN113325109 A CN 113325109A
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lincomycin
mushroom dregs
detecting
residual quantity
standard
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王�义
张鹏
金昌福
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Ningxia Xiwang Tianye Biological Agricultural Technology Co ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material

Abstract

The invention discloses a method for detecting residual quantity of lincomycin in mushroom dregs, which comprises the steps of preparing a reference substance solution and a test substance solution, detecting by adopting a high performance liquid chromatography, injecting the standard substance solution and the test substance solution into a liquid chromatograph, and calculating the titer of lincomycin according to an external standard method. The invention establishes a high performance liquid chromatography detection analysis method for lincomycin in mushroom dregs by optimizing chromatographic conditions and testing the preparation methods of a test sample and a standard substance; a method for detecting lincomycin in mushroom dregs is established by optimizing chromatographic conditions and a purification process, and proved by methodological verification test research: the established method has high accuracy, strong specificity and good reproducibility, and can effectively detect the residual lincomycin in the mushroom dregs.

Description

Method for detecting residual quantity of lincomycin in mushroom dregs
Technical Field
The invention relates to the technical field of antibiotic detection, in particular to a method for detecting residual quantity of lincomycin in mushroom dregs.
Background
At present, antibiotic medicines are widely applied, the main application mode is as veterinary medicines, and the detection is mainly focused on animal-derived foods. The main detection methods comprise high performance liquid chromatography, high performance liquid chromatography-tandem mass spectrometry, capillary electrophoresis and enzyme linked immunosorbent assay.
The antibiotic dregs are the by-products in the process of producing antibiotics by fermentation, and mainly comprise fermentation mycelium, saccharides, crude protein, a small amount of inorganic salt which is not completely utilized, and antibiotics which are not completely extracted and metabolites thereof. The appearance is like bean curd residue, the odor is different due to different cultured fungi, the water content is generally higher, and the bean curd residue is easy to be stacked and stored for secondary fermentation to generate odor gas. In the process of producing lincomycin by microbial fermentation, a large amount of lincomycin is remained in the mushroom dregs due to low extraction rate and is extremely difficult to degrade, thereby causing serious environmental pollution. According to relevant data statistics, the annual discharge amount of lincomycin in China is about millions of tons, and the current main treatment mode is land occupation stacking. The lincomycin bacterial residues are earthy blue in appearance, the water content is 70-85%, and stacking treatment not only causes resource waste, but also pollutes ecological environments such as soil, underground water and the like after being washed by rainwater. In the past, the fungus dregs are dried and processed to be used as feed or feed additives. However, as a result of recent research, residual antibiotics in the mushroom dregs accumulate in animals, and human beings eating the animal-derived food can cause harm to the bodies. And the animals can generate drug resistance to the antibiotics after long-term use of the antibiotics, induce generation of drug-resistant bacteria and destroy the micro-ecological balance of the environment. In 2008, the antibiotic residues are listed in dangerous waste lists in China, and the antibiotic residues are not subjected to harmless treatment and are strictly prohibited from secondary utilization. A stable, sensitive and efficient method for detecting the residual quantity of the lincomycin in the mushroom dregs is established, and a foundation is laid for establishing a mushroom dreg pollution control standard.
The detection of the residual quantity of the antibiotics in the mycelium is earlier in foreign research, and mainly detects the content of the penicillin in the penicillin fermentation intermediate product. The method for detecting lincomycin in mushroom dregs reported in China at present is a microbial culture method, the sensitivity of the method is low, the method is incomplete, the accuracy, precision and detection limit of the method are all considered, and the requirement of modern residue detection analysis cannot be met. Therefore, accurate and reliable residual detection methods have yet to be discussed.
Disclosure of Invention
The invention aims to make up the defect that lincomycin in lincomycin bacterial residues cannot be quickly/accurately detected in the prior art, and does not solve the problem of influence of matrix effect effectively, so that a method for extracting and measuring the residual quantity of lincomycin in lincomycin bacterial residues is provided, and a method basis is provided for detecting the residual quantity and transformation of lincomycin in lincomycin bacterial residues.
The invention discloses a method for detecting residual quantity of lincomycin in mushroom dregs, which is carried out according to the following steps:
firstly, preparing a sample to be tested:
1) weighing the lincomycin-containing fungi residues, adding an ammoniated acetonitrile extractant with the volume percentage of 0.1-0.15%, performing vortex oscillation for 1min, performing auxiliary extraction in ultrasound for 30min, centrifuging at 3000-4000 rpm for 10min, and taking supernatant;
2) weighing PSA and C18And anhydrous Na2SO4Adding the supernatant of the previous step after vortex mixing for 1min, continuing vortex for 1min, centrifuging at 4000rpm/min for 10min, and collecting the supernatant to obtain a test solution;
secondly, drawing a standard curve:
diluting lincomycin standard stock solution into standard working solutions with mass concentrations of 10.00mg/L, 20.00mg/L, 40.00mg/L, 50mg/L, 100.00mg/L, 200.00mg/L and 400mg/L by using methanol; detecting the standard working solution by adopting a high performance liquid chromatography, drawing a standard curve by taking the measured peak area as a vertical coordinate and the concentration of the standard working solution as a horizontal coordinate, and solving a regression equation and a correlation coefficient;
thirdly, determination: sucking the standard substance working solution and the sample solution, injecting the standard substance working solution and the sample solution into a liquid chromatograph, and calculating the residual quantity of lincomycin according to an external standard method;
chromatographic conditions are as follows: a chromatographic column: Aglientextend-C18Column, inner diameter of chromatographic column 4.6mm, length of column 250mm, diameter of packing particle 5 μm, mobile phase: methanol-0.05 moL/L sodium tetraborate decahydrateThe compound is mixed solution according to the volume ratio of 60:40, and the detection wavelength is as follows: 214nm, sample size: 10 μ L, flow rate: 1mL/min, column temperature: at 30 ℃.
The invention has the following beneficial effects:
the method for measuring the lincomycin residues in the lincomycin residues is simple and convenient to operate, high in accuracy, good in linear relation between the lincomycin content and the peak area, and capable of meeting the requirements of residue analysis on the recovery rate, the sensitivity, the detection limit, the relative standard deviation and the like. Experiments prove that the method can be used for various lincomycin bacterial residues with larger property differences, and the recovery rate, the sensitivity, the detection limit and the like of the lincomycin bacterial residues have better accuracy and precision in each batch of bacterial residues.
The method can effectively extract lincomycin from the mushroom dregs and reduce the influence of other impurities in the mushroom dregs on subsequent detection as much as possible, thereby improving the accuracy of the detection
(1) The invention provides a high performance liquid chromatography method for extracting lincomycin from lincomycin mushroom dregs by combining ultrasonic assistance with a dispersion solid phase extraction method, which is more perfect for the first time: the method comprises the steps of extracting lincomycin from lincomycin residues in an ultrasonic-assisted manner, applying a dispersed solid phase extraction technology to extract purification, and applying a high performance liquid chromatography-ultraviolet detector to lincomycin content determination.
(2) The method has high sensitivity, can meet the detection requirement of China on the highest residue limit of the lincomycin in animal tissues, and can provide a certain technical basis for the resource utilization of the lincomycin bacterial residues for the feed.
The recovery rate of the lincomycin in the method is 82-115% at the addition concentration level of 100-800 mg/kg. The limit of qualitative detection is 0.027mg/kg, and the limit of quantitative detection is 0.089 mg/kg. The variation coefficient in the day is 3-9 percent and is less than 10 percent; the diurnal variation coefficient is 7.5-12% and less than 15%.
Drawings
FIG. 1 is a lincomycin standard curve;
FIG. 2 is a standard chromatogram of lincomycin at a concentration of 100 mg/L;
FIG. 3 is a chromatogram of residual lincomycin in fresh lincomycin bacterial residue.
Detailed Description
The first embodiment is as follows: the method for detecting the residual quantity of lincomycin in the mushroom dregs in the embodiment is carried out according to the following steps:
firstly, preparing a sample to be tested:
1) weighing lincomycin-containing fungi residues, adding an extracting agent, carrying out vortex oscillation for 1min, carrying out auxiliary extraction in ultrasound for 30min, centrifuging at 3000-4000 rpm for 10min, and taking supernatant;
2) weighing PSA and C18And anhydrous Na2SO4Adding the supernatant of the previous step after vortex mixing for 1min, continuing vortex for 1min, centrifuging at 4000rpm/min for 10min, and collecting the supernatant to obtain a test solution;
secondly, drawing a standard curve:
diluting lincomycin standard stock solution into standard working solutions with mass concentrations of 10.00mg/L, 20.00mg/L, 40.00mg/L, 50mg/L, 100.00mg/L, 200.00mg/L and 400mg/L by using methanol; detecting the standard working solution by adopting a high performance liquid chromatography, drawing a standard curve by taking the measured peak area as a vertical coordinate and the concentration of the standard working solution as a horizontal coordinate, and solving a regression equation and a correlation coefficient;
thirdly, determination: sucking the standard substance working solution and the sample solution, injecting the standard substance working solution and the sample solution into a liquid chromatograph, and calculating the residual quantity of lincomycin according to an external standard method;
chromatographic conditions are as follows: a chromatographic column: Aglientextend-C18Column, inner diameter of chromatographic column 4.6mm, length of column 250mm, diameter of packing particle 5 μm, mobile phase: the detection wavelength of a solution mixed by methanol-0.05 moL/L sodium tetraborate decahydrate according to the volume ratio of 60:40 is as follows: 214nm, sample size: 10 μ L, flow rate: 1mL/min, column temperature: at 30 ℃.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the mass volume ratio of the lincomycin bacterial residues to the extracting agent is 1 g: 5-15 mL. The rest is the same as the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the mass volume ratio of the lincomycin bacterial residues to the extracting agent is 1 g: 10 mL. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the extractant is ammoniated acetonitrile with the volume percentage content of 0.1 percent to 0.15 percent. The rest is the same as the first embodiment.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the extractant is ammoniated acetonitrile with the volume percentage content of 0.12 percent. The rest is the same as the first embodiment.
The sixth specific implementation mode: the first difference between the present embodiment and the specific embodiment is: PSA, C18And anhydrous Na2SO4The mass-to-volume ratio of (A) is 0.05-0.1 g: 1.0 g: 10 mL. The rest is the same as the first embodiment.
The seventh embodiment: the first difference between the present embodiment and the specific embodiment is: PSA, C18And anhydrous Na2SO4The mass-to-volume ratio of (2) is 0.05 g: 1.0 g: 10 mL. The rest is the same as the first embodiment.
The specific implementation mode is eight: the first difference between the present embodiment and the specific embodiment is: anhydrous Na in step two2SO4And the volume ratio of the added supernatant liquid is 10: 4. the rest is the same as the first embodiment.
The specific implementation method nine: the first difference between the present embodiment and the specific embodiment is: the residual quantity of lincomycin in the mushroom dregs is 800-850 mg/Kg. The rest is the same as the first embodiment.
The detailed implementation mode is ten: the first difference between the present embodiment and the specific embodiment is: the residual quantity of lincomycin in the mushroom dregs is 800-820 mg/Kg. The rest is the same as the first embodiment.
The concrete implementation mode eleven: the first difference between the present embodiment and the specific embodiment is: the limit of qualitative detection and quantitative detection of the method is 0.027mg/kg and 0.089 mg/kg. The rest is the same as the first embodiment.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1
The method for detecting the residual titer of the lincomycin in the mushroom dregs comprises the following steps:
the instrument comprises the following steps: high performance liquid chromatograph
Chromatographic conditions are as follows: the chromatographic column is Aglientextend-C18Column (4.6mm × 250mm,5 μm), mobile phase: methanol-0.05 moL/L sodium tetraborate decahydrate 60:40, detection wavelength: 214nm, sample size: 10 μ L, flow rate: 1mL/min, column temperature: at 30 ℃.
1) Preparing a sample to be tested: weighing 1g (accurate to 0.0001g) of sample, adding 10mL of an extracting agent (012% ammoniated acetonitrile) into a 50mL polypropylene centrifuge tube, carrying out vortex oscillation for 1min, carrying out auxiliary extraction in ultrasound for 30min, centrifuging at 3000-4000 rpm for 10min, and taking supernatant. 50mgPSA, 94mgC are accurately weighed18And 1.0g of anhydrous Na2SO4And (3) mixing in a 10mL polypropylene centrifuge tube by vortex for 1min, adding 4mL of supernatant, continuing to vortex for 1min, centrifuging at 4000rpm/min for 10min, transferring 1.0mL of supernatant, and waiting for detection on a machine.
2) Drawing a standard curve: diluting the standard stock solution with methanol to standard solutions with mass concentrations of 10.0mg/L, 20.0mg/L, 40.0mg/L, 50.0mg/L, 100.0mg/L, 200.0mg/L and 400.0mg/L, detecting the standard working solution by high performance liquid chromatography, taking the measured peak area as ordinate, taking the corresponding standard solution concentration as abscissa, drawing a standard curve, and solving a regression equation and a correlation coefficient.
3) And (3) determination: and sucking 10 microlitres of each of the standard solution and the sample solution, injecting into a liquid chromatograph, and analyzing and detecting.
4) And (3) calculating: and calculating the peak area corresponding to the separated lincomycin, and carrying out quantitative calculation according to the standard curve to obtain the lincomycin content.
5) Method recovery, detection limit and quantitation limit: and (3) detecting the recovery rate of the method by adopting a standard recovery method, adding 100, 400 and 800mg/kg lincomycin standard substance solutions into the mushroom dregs, detecting the lincomycin content by using the method, and calculating the recovery rate of the method. The limit of detection is determined by 3 times the signal-to-noise ratio and the limit of quantitation is determined by 10 times the signal-to-noise ratio. The experimental result shows that the recovery rate of the method is 82-115%, the limit of qualitative detection is 0.027mg/kg, and the limit of quantitative detection is 0.089 mg/kg.
Example 2
The method for detecting the residual lincomycin in the mushroom dregs comprises the following steps:
the instrument comprises the following steps: high performance liquid chromatograph
Chromatographic conditions are as follows: the chromatographic column is Aglientextend-C18Column (4.6mm × 250mm,5 μm), mobile phase: methanol-0.05 moL/L sodium tetraborate decahydrate 60:40, detection wavelength: 214nm, sample size: 10 μ L, flow rate: 1mL/min, column temperature: at 30 ℃.
1) Preparing a sample to be tested: weighing 1g (accurate to 0.0001g) of sample, adding 10mL of an extracting agent (012% ammoniated acetonitrile) into a 50mL polypropylene centrifuge tube, carrying out vortex oscillation for 1min, carrying out auxiliary extraction in ultrasound for 30min, centrifuging at 3000-4000 rpm for 10min, and taking supernatant. 50mgPSA, 94mgC are accurately weighed18And 1.0g of anhydrous Na2SO4And (3) mixing in a 10mL polypropylene centrifuge tube by vortex for 1min, adding 4mL of supernatant, continuing to vortex for 1min, centrifuging at 4000rpm/min for 10min, transferring 1.0mL of supernatant, and waiting for detection on a machine.
2) Drawing a standard curve: diluting the standard stock solution with methanol to standard solutions with mass concentrations of 10.00mg/L, 20.0mg/L, 40.0mg/L, 50.0mg/L, 100.0mg/L, 200.0mg/L and 400.0mg/L, detecting the standard working solution by high performance liquid chromatography, taking the measured peak area as ordinate, taking the corresponding standard solution concentration as abscissa, drawing a standard curve, and solving a regression equation and a correlation coefficient.
3) And (3) determination: sucking 10 μ L of the standard solution and the sample solution, injecting into a liquid chromatograph, and analyzing and detecting.
4) And (3) calculating: and calculating the peak area corresponding to the separated lincomycin, and carrying out quantitative calculation according to the standard curve to obtain the lincomycin content.
5) Method recovery, detection limit and quantitation limit: and (3) detecting the recovery rate of the method by adopting a standard recovery method, adding 100, 400 and 800mg/kg lincomycin standard substance solutions into the mushroom dregs, detecting the lincomycin content by using the method, and calculating the recovery rate of the method. The limit of detection is determined by 3 times the signal-to-noise ratio and the limit of quantitation is determined by 10 times the signal-to-noise ratio. The experimental result shows that the recovery rate of the method is 82-115%, the limit of qualitative detection is 0.027mg/kg, and the limit of quantitative detection is 0.089 mg/kg.
The method comprises the following steps:
the standard adding concentrations in the lincomycin bacterial residue samples are respectively 100 mg/kg, 400 mg/kg and 800 mg/kg. The experimental method is adopted for analysis and detection, the laboratory is repeated for 3 times, the obtained recovery rate and the standard deviation thereof are obtained, and the lincomycin content in the sample is calculated according to the formula (1).
Figure BDA0003099224320000061
In the formula: x-lincomycin content in milligrams per kilogram (mg/kg) of the sample;
c-concentration of lincomycin in the sample solution in milligrams per liter (mg/L);
m is the sample mass in grams (g);
v-volume of sample solution in milliliters (mL)
The recovery rate of the lincomycin in the method is 82-115% at the addition concentration level of 100-800 mg/kg. The limit of qualitative detection is 0.027mg/kg, and the limit of quantitative detection is 0.089 mg/kg. The variation coefficient in the day is 3-9 percent and is less than 10 percent; the diurnal variation coefficient is 7.5-12% and less than 15%.

Claims (9)

1. A method for detecting residual quantity of lincomycin in mushroom dregs comprises the following steps:
firstly, preparing a sample to be tested:
1) weighing the lincomycin-containing fungi residues, adding an ammoniated acetonitrile extractant with the volume percentage of 0.1-0.15%, performing vortex oscillation for 1min, performing auxiliary extraction in ultrasound for 30min, centrifuging at 3000-4000 rpm for 10min, and taking supernatant;
2) weighing PSA and C18And anhydrous Na2SO4Adding the supernatant of the previous step after vortex mixing for 1min, continuing vortex for 1min, centrifuging at 4000rpm/min for 10min, and collecting the supernatant to obtain a test solution;
secondly, drawing a standard curve:
diluting lincomycin standard stock solution into standard working solutions with mass concentrations of 10.00mg/L, 20.00mg/L, 40.00mg/L, 50mg/L, 100.00mg/L, 200.00mg/L and 400mg/L by using methanol; detecting the standard working solution by adopting a high performance liquid chromatography, drawing a standard curve by taking the measured peak area as a vertical coordinate and the concentration of the standard working solution as a horizontal coordinate, and solving a regression equation and a correlation coefficient;
thirdly, determination: sucking the standard substance working solution and the sample solution, injecting the standard substance working solution and the sample solution into a liquid chromatograph, and calculating the residual quantity of lincomycin according to an external standard method;
chromatographic conditions are as follows: a chromatographic column: Aglientextend-C18Column, inner diameter of chromatographic column 4.6mm, length of column 250mm, diameter of packing particle 5 μm, mobile phase: the detection wavelength of a solution mixed by methanol-0.05 moL/L sodium tetraborate decahydrate according to the volume ratio of 60:40 is as follows: 214nm, sample size: 10 μ L, flow rate: 1mL/min, column temperature: at 30 ℃.
2. The method for detecting the residual quantity of the lincomycin in the mushroom dregs as claimed in claim 1, wherein the mass volume ratio of the lincomycin mushroom dregs to the extracting agent is 1 g: 5-15 mL.
3. The method for detecting the residual quantity of the lincomycin in the mushroom dregs as claimed in claim 1 or 2, wherein the mass-volume ratio of the lincomycin mushroom dregs to the extracting agent is 1 g: 10 mL.
4. The method for detecting the residual quantity of lincomycin in mushroom dregs as claimed in claim 1, wherein the extracting agent is ammoniated acetonitrile with a volume percentage of 0.12%.
5. The method for detecting the residual quantity of lincomycin in mushroom dregs according to claim 1, wherein PSA and C are18And anhydrous Na2SO4The mass-to-volume ratio of (A) is 0.05-0.1 g: 1.0 g: 10 mL.
6. The method for detecting the residual quantity of lincomycin in mushroom dregs according to claim 1 or 5, wherein PSA and C are18And anhydrous Na2SO4The mass-to-volume ratio of (2) is 0.05 g: 1.0 g: 10 mL.
7. The method for detecting the residual quantity of lincomycin in mushroom dregs according to claim 1, wherein anhydrous Na is adopted in the second step2SO4And the volume ratio of the added supernatant liquid is 10: 4.
8. the method for detecting the residual quantity of lincomycin in mushroom dregs according to claim 1, wherein the residual quantity of lincomycin in mushroom dregs is 800-850 mg/Kg.
9. The method for detecting the residual quantity of lincomycin in mushroom dregs according to claim 8, wherein the residual quantity of lincomycin in mushroom dregs is 800-820 mg/Kg.
CN202110629137.3A 2017-12-29 2017-12-29 Method for detecting residual quantity of lincomycin in mushroom dregs Pending CN113325109A (en)

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