CN112198264A - Method for detecting veterinary drug residues in bear gall powder - Google Patents
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Abstract
The invention relates to the technical field of medicinal material safety detection, in particular to a method for detecting veterinary drug residues in bear gall powder, which is characterized by comprising the following steps of; s1, preparation of control stock solution: precisely weighing appropriate amount of each reference substance, and adding appropriate solvent to obtain solution containing 100 μ g per 1ml according to solubility to obtain 100 μ g/ml reference substance stock solution; s2, preparation of mixed control solution: precisely measuring a proper amount of the reference substance stock solution, and preparing a solution containing 1 mu g of reference substance per ml by using 15% acetonitrile to obtain a mixed reference substance solution of 1 mu g/ml. According to the invention, the method for detecting the veterinary drug residues in the bear gall powder can comprehensively detect the 169 veterinary drug residues in the bear gall powder, so that the problems of side effects of anaphylactic reaction caused by the veterinary drug and drug resistance generated by a human body are solved, meanwhile, the method is simple, convenient and quick, the working efficiency can be improved, and the detection cost can be reduced.
Description
Technical Field
The invention relates to the technical field of medicinal material safety detection, in particular to a method for detecting veterinary drug residues in bear gall powder.
Background
The bear gall is used as a traditional rare Chinese medicinal material, and before the 80 th century, the gall bladder with the bile is taken by killing a bear, and the bile is dried to form an agglomeration. Since the beginning of the 80 s, scientific researches are continuously carried out by introducing technologies, and a series of technologies such as artificial black bear feeding, artificial propagation, live bear gall taking, ductless drainage and the like are established. Wherein, through the no pipe drainage technique, the misery of black bear has been eliminated greatly, has promoted the development of black bear aquaculture. Because of the contradiction between the insufficient supply of bear gall powder market and market demand, domestic bear raising enterprises and pharmaceutical enterprises continuously improve the yield of bear gall powder through technical improvement.
In the black bear breeding process, part of bear raising enterprises reach the black bear specified by the forestry department and can perform artificial bile drainage, and the bile drainage is performed after the fistulization wound is completely healed for the first time. If the black bear needs to be treated by using medicines during the illness period, the black bear is treated by adopting traditional Chinese medicines as much as possible, bile collection is not carried out during the illness period of the black bear, and bile drainage is carried out after the black bear is completely healthy.
Enterprises need to use narcotics and antibiotics in the self-fistulization ductless drainage operation of black bears. The antibiotic is used for feeding treatment after the operation. The medicines used in the black bear operation period include anesthetic seralazine hydrochloride injection, antibiotics include penicillin sodium for injection, streptomycin sulfate for injection, benzathine for injection, etamsylate injection, vitamin C injection, and the like, and the medicines used in the postoperative recovery period include levofloxacin hydrochloride tablets and the like.
After the black bear uses the veterinary drug, the drug is accumulated or stored in animal tissues or organs, and the drug enters bear bile through a metabolic pathway, and the bear bile enters bear bile through processing to be prepared into traditional Chinese medicine bear bile powder which is put into the drug production process to be prepared into Chinese patent medicine. Some veterinary drugs have side effects of causing anaphylactic reaction, causing drug resistance of human bodies and the like, so the detection of the veterinary drug residues in the bear gall powder has important significance for ensuring the drug safety.
In summary, the present invention provides a method for detecting veterinary drug residues in bear gall powder to solve the existing problems.
Disclosure of Invention
The invention aims to provide a method for detecting veterinary drug residues in bear gall powder, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for detecting veterinary drug residues in bear gall powder comprises the following steps:
s1, preparation of control stock solution: precisely weighing appropriate amount of each reference substance, and adding appropriate solvent to obtain solution containing 100 μ g per 1ml according to solubility to obtain 100 μ g/ml reference substance stock solution;
s2, preparation of mixed control solution: precisely measuring a proper amount of a reference substance stock solution, and preparing a solution containing 1 mu g of reference substance per ml by using 15% acetonitrile to obtain a mixed reference substance solution of 1 mu g/ml;
s3, preparation of matrix mix control solution: taking a proper amount of blank bear gall powder samples, grinding, uniformly mixing, precisely weighing about 0.1g of the blank bear gall powder samples, placing the obtained product into a 50ml polystyrene centrifuge tube with a plug, precisely adding 100 mu l of mixed reference substance solution, and processing the obtained product with the preparation method of the test substance solution to obtain the test sample solution;
s4, preparation of a test solution: taking a proper amount of bear gall powder sample, grinding, mixing uniformly, taking about 0.1g, precisely weighing, placing in a 50ml polystyrene centrifuge tube with a plug, adding 0.1mol/L Na2EDTA-McIlvaine buffer solution and 10ml of buffer solution (pH4.0), shaking uniformly, and vortexing to fully infiltrate. Precisely adding 10ml of 5% glacial acetic acid acetonitrile, uniformly mixing by vortex, and placing on an oscillator to violently shake for 10 minutes; adding 5g of anhydrous sodium chloride-sodium sulfate mixed powder according to a certain proportion, placing on an oscillator, oscillating for 3 minutes violently, centrifuging for 5 minutes, and layering; sucking 6ml of supernatant, placing the supernatant into a dispersed solid phase extraction purification tube which is pre-filled with a purification material, vortexing to fully mix the supernatant, placing the supernatant on an oscillator to violently oscillate for 5 minutes to completely purify the supernatant, centrifuging the supernatant for 5 minutes, precisely sucking 2ml of supernatant, placing the supernatant on a nitrogen blowing instrument to concentrate the supernatant in a water bath at 40 ℃ until the supernatant is dry, precisely adding 0.2ml of 15% acetonitrile, vortexing the supernatant for 1 minute, performing ultrasonic treatment for 1 minute, mixing the supernatant evenly, centrifuging the mixture, and taking the supernatant to obtain the product;
s5, assay: precisely sucking 1 μ l of the matrix mixed reference solution and sample solution respectively, injecting into a liquid chromatogram-mass spectrometer, and measuring.
Preferably, the S5, liquid chromatography includes a mobile phase and an elution mode, and the mobile phase in the S5, liquid chromatography is any one of the following (1) to (4):
(1) mobile phase a 0.1% formic acid (containing 0.2mmol/L ammonium formate and 0.2mmol ammonium fluoride) solution-mobile phase B0.1% formic acid in acetonitrile;
(2) mobile phase a 0.2% formic acid (containing 0.3mmol/L ammonium formate and 0.3mmol ammonium fluoride) solution-mobile phase B0.1% formic acid in acetonitrile;
(3) mobile phase a 0.2% formic acid (containing 0.5mmol/L ammonium formate and 0.5mmol ammonium fluoride) solution-mobile phase B0.2% formic acid in acetonitrile;
(4) mobile phase a 0.1% formic acid (containing 0.4mmol/L ammonium formate and 0.4mmol ammonium fluoride) solution-mobile phase B0.2% formic acid in acetonitrile.
S5, adopting gradient elution in the liquid chromatography, wherein the flow of the gradient elution is any one of the following (1) to (3):
(1) 0-1.5 min, 1% of mobile phase B by volume percentage, 1.5-2.0 min, 1-10% of mobile phase B by volume percentage, 2.0-4.5 min, 10-18% of mobile phase B by volume percentage, 4.5-6 min, 18-22% of mobile phase B by volume percentage, 6-9 min, 22-30% of mobile phase B by volume percentage, 9-12 min and 30-35% of mobile phase B by volume percentage; 12-20 min, 35-80% of mobile phase B by volume percentage, 20-26 min, 80-100% of mobile phase B by volume percentage;
(2) 0-0.5 min, 2% of mobile phase B by volume percentage, 0.5-1.8 min, 2-15% of mobile phase B by volume percentage, 1.8-3.5 min, 10-15% of mobile phase B by volume percentage, 3.5-6 min, 15-25% of mobile phase B by volume percentage, 6-7 min, 25-30% of mobile phase B by volume percentage, 7-11 min and 30-35% of mobile phase B by volume percentage; 11-16 min, 35-100% of mobile phase B by volume percentage concentration, 16-26 min and 100% of mobile phase B by volume percentage concentration;
(3) 0-1.0 min, 3% of mobile phase B by volume percentage, 0.5-1.8 min, 2-15% of mobile phase B by volume percentage, 1.8-5 min, 10-15% of mobile phase B by volume percentage, 5-10 min, 15-20% of mobile phase B by volume percentage, 10-15 min, 20-30% of mobile phase B by volume percentage, 15-20 min and 30-35% of mobile phase B by volume percentage; 20-30 min, 35-100% of mobile phase B by volume percentage concentration, 30-35 min and 100% of mobile phase B by volume percentage concentration.
In the S5, in the mass spectrometry condition, the instrument adopts a triple quadrupole mass spectrometer, and Multiple Reaction Monitoring (MRM) is performed in an electrospray ionization (ESI) mode.
Preferably, the S4, 0.1mol/L Na2EDTA-McIlvaine buffer solution (pH4.0) preparation method comprises the following steps: 2.9g of citric acid monohydrate, 10.9g of disodium hydrogen phosphate dodecahydrate and 37.2g of disodium ethylene diamine tetraacetate dihydrate were weighed, water was added to 900ml, pH was adjusted to 4.0 with 1mol/L of sodium hydroxide solution, and volume was determined to 1L with water.
Preferably, the purification material of S4 is magnesium sulfate 300mg, octadecylsilane chemically bonded silica 300mg, and N-Propylethylenediamine (PSA)1800 mg.
Preferably, in S4, the vibration frequency of the vigorous oscillation is 500 times/min.
Preferably, in the step S4, anhydrous sodium chloride and sodium sulfate are added in a ratio of 1: 4.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the method for detecting the veterinary drug residues in the bear gall powder can comprehensively detect the 169 veterinary drug residues in the bear gall powder, so that the problems of side effects of anaphylactic reaction caused by the veterinary drug and drug resistance generated by a human body are solved, meanwhile, the method is simple, convenient and quick, the working efficiency can be improved, and the detection cost can be reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention provides a technical scheme that: a method for detecting veterinary drug residues in bear gall powder comprises the following steps:
s1, preparation of control stock solution: precisely weighing appropriate amount of each reference substance, and adding appropriate solvent to obtain solution containing 100 μ g per 1ml according to solubility to obtain 100 μ g/ml reference substance stock solution;
s2, preparation of mixed control solution: precisely measuring a proper amount of a reference substance stock solution, and preparing a solution containing 1 mu g of reference substance per ml by using 15% acetonitrile to obtain a mixed reference substance solution of 1 mu g/ml;
s3, preparation of matrix mix control solution: taking a proper amount of blank bear gall powder samples, grinding, uniformly mixing, precisely weighing about 0.1g of the blank bear gall powder samples, placing the obtained product into a 50ml polystyrene centrifuge tube with a plug, precisely adding 100 mu l of mixed reference substance solution, and processing the obtained product with the preparation method of the test substance solution to obtain the test sample solution;
s4, preparation of a test solution: taking a proper amount of bear gall powder sample, grinding, mixing uniformly, taking about 0.1g, precisely weighing, placing in a 50ml polystyrene centrifuge tube with a plug, adding 0.1mol/L Na2EDTA-McIlvaine buffer solution and 10ml of buffer solution (pH4.0), shaking uniformly, and vortexing to fully infiltrate. Precisely adding 10ml of 5% glacial acetic acid acetonitrile, uniformly mixing by vortex, and placing on an oscillator to violently shake for 10 minutes; adding 5g of anhydrous sodium chloride-sodium sulfate mixed powder according to a certain proportion, placing on an oscillator, oscillating for 3 minutes violently, centrifuging for 5 minutes, and layering; sucking 6ml of supernatant, placing the supernatant into a dispersed solid phase extraction purification tube which is pre-filled with a purification material, vortexing to fully mix the supernatant, placing the supernatant on an oscillator to violently oscillate for 5 minutes to completely purify the supernatant, centrifuging the supernatant for 5 minutes, precisely sucking 2ml of supernatant, placing the supernatant on a nitrogen blowing instrument to concentrate the supernatant in a water bath at 40 ℃ until the supernatant is dry, precisely adding 0.2ml of 15% acetonitrile, vortexing the supernatant for 1 minute, performing ultrasonic treatment for 1 minute, mixing the supernatant evenly, centrifuging the mixture, and taking the supernatant to obtain the product;
s5, assay: precisely sucking 1 μ l of the matrix mixed reference solution and sample solution respectively, injecting into a liquid chromatogram-mass spectrometer, and measuring.
Example (b):
1. instrument and reagent
Agilent Zorbax Eclipse plus C18(3.0 x 150mm, 1.8 μm) was used as a column. The chromatographic conditions used were: taking a 0.2% formic acid (containing 0.5mmol/L ammonium formate and 0.5mmol ammonium fluoride) solution as a mobile phase A, and taking a 0.2% formic acid acetonitrile solution as a mobile phase B; the column temperature was 40 ℃ and the flow rate was 0.5 ml/min.
TABLE 1 gradient of mobile phase
| Time (min) | A(％) | B(％) |
| 0 | 98 | 2 |
| 0.5 | 98 | 2 |
| 1.8 | 85 | 10 |
| 3.5 | 80 | 15 |
| 6 | 75 | 25 |
| 7 | 70 | 30 |
| 11 | 65 | 35 |
| 16 | 0 | 100 |
| 26 | 0 | 100 |
Mass spectrum conditions: multiple Reaction Monitoring (MRM) in electrospray ionization (ESI) mode using a triple quadrupole mass spectrometer detector, the monitored ion pairs are shown in table 2.
TABLE 2 Mass Spectrometry conditions for the Compounds
The method comprises the following steps: preparation of a control stock solution (100. mu.g/ml): precisely weighing appropriate amount of each reference substance, and adding appropriate solvent (shown in Table 1) according to solubility to obtain solution containing 100 μ g per 1 ml.
Step two: preparation of Mixed control solution (1. mu.g/ml): precisely measuring a proper amount of a reference substance stock solution (100 mu g/ml), and preparing a solution containing 1 mu g of reference substance stock solution per ml by using 15% acetonitrile.
Step three: preparation of matrix mix control solution: taking a proper amount of blank bear gall powder samples (the 169 veterinary drug residues are not detected), grinding, uniformly mixing, taking about 0.1g, precisely weighing, placing in a 50ml polystyrene centrifuge tube with a plug, precisely adding 100 mu l of mixed reference substance solution (1 mu g/ml), and processing with the preparation method of the test sample solution to obtain the bear gall powder.
Step four: preparation of a test solution: taking a proper amount of bear gall powder sample, grinding, mixing uniformly, taking about 0.1g, precisely weighing, placing in a 50ml polystyrene centrifuge tube with a plug, adding 10ml of 0.1mol/L Na2EDTA-McIlvaine buffer solution (pH4.0), shaking uniformly, and vortexing to fully infiltrate. Add precisely 10ml of 5% glacial acetic acid acetonitrile, vortex to mix well, place on shaker shake vigorously (500 times/min) for 10 min. 5g of a mixed powder of anhydrous sodium chloride and sodium sulfate (1:4) was added thereto, followed by shaking vigorously on a shaker for 3 minutes and centrifugation for 5 minutes to separate layers. Absorbing 6ml of supernatant, placing the supernatant into a dispersed solid phase extraction purification tube (magnesium sulfate 300mg, octadecylsilane chemically bonded silica gel 300mg, N-Propylethylenediamine (PSA)1800 mg) which is pre-filled with purification materials, vortexing to fully mix the supernatant, placing the mixture on an oscillator to oscillate vigorously for 5 minutes (500 times/minute) to completely purify the mixture, centrifugating for 5 minutes, precisely absorbing 2ml of supernatant, placing the mixture on a nitrogen blowing instrument to concentrate the mixture to be dry in a water bath at 40 ℃, precisely adding 0.2ml of 15% acetonitrile, vortexing for 1 minute, ultrasonically mixing for 1 minute, uniformly mixing, centrifugating, and taking the supernatant to obtain the product.
Step five: the determination method comprises the following steps: precisely sucking 1 μ l of the matrix mixed reference solution and sample solution respectively, injecting into a liquid chromatogram-mass spectrometer, and measuring. If the sample solution detects a chromatographic peak with the same retention time as the reference substance, and the selected ion abundance ratio and the ion abundance ratio of the reference substance solution with the corresponding concentration meet the specification of the following table, it can be determined that the sample solution has the component.
3. Methodology validation
(1) Specificity test: taking a proper amount of blank bear gall powder samples, grinding, mixing uniformly, taking about 0.1g, precisely weighing, placing in a 50ml polystyrene centrifuge tube with a plug, processing with the preparation method of the test sample solution, and carrying out sample injection and measurement. The results did not detect the 169 veterinary drug residues, indicating that the blank matrix did not interfere with the assay.
(2) Detection limit test: taking a proper amount of blank bear gall powder samples, grinding, mixing uniformly, taking about 0.1g, weighing in seven copies precisely, placing in a 50ml polystyrene centrifuge tube with a plug, respectively adding precisely 1 mul, 10 mul, 50 mul, 100 mul, 250 mul, 500 mul and 1000 mul of mixed reference substance solution (100ng/ml), processing with the preparation method of the test substance solution, injecting and measuring. The detection limit was determined by visual evaluation using the true minimum detection concentration. As a result, the detection limit of the 169 compounds was 1 to 1000. mu.g/kg, which is shown in Table 1.
(3) And (3) repeatability test: a reproducible test was carried out at the loading level (1000. mu.g/kg), and 169 veterinary drugs were detected in each case in six replicates.
Table 1 selected 169 veterinary drugs
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A method for detecting veterinary drug residues in bear gall powder is characterized by comprising the following steps:
s1, preparation of control stock solution: precisely weighing appropriate amount of each reference substance, and adding appropriate solvent to obtain solution containing 100 μ g per 1ml according to solubility to obtain 100 μ g/ml reference substance stock solution;
s2, preparation of mixed control solution: precisely measuring a proper amount of a reference substance stock solution, and preparing a solution containing 1 mu g of reference substance per ml by using 15% acetonitrile to obtain a mixed reference substance solution of 1 mu g/ml;
s3, preparation of matrix mix control solution: taking a proper amount of blank bear gall powder samples, grinding, uniformly mixing, precisely weighing about 0.1g of the blank bear gall powder samples, placing the obtained product into a 50ml polystyrene centrifuge tube with a plug, precisely adding 100 mu l of mixed reference substance solution, and processing the obtained product with the preparation method of the test substance solution to obtain the test sample solution;
s4, preparation of a test solution: taking a proper amount of bear gall powder sample, grinding, uniformly mixing, taking about 0.1g, precisely weighing, placing in a 50ml polystyrene centrifuge tube with a plug, adding 0.1mol/L Na2EDTA-McIlvaine buffer solution and 10ml of buffer solution (pH4.0), shaking uniformly, and vortexing to fully infiltrate; precisely adding 10ml of 5% glacial acetic acid acetonitrile, uniformly mixing by vortex, and placing on an oscillator to violently shake for 10 minutes; adding 5g of anhydrous sodium chloride-sodium sulfate mixed powder according to a certain proportion, placing on an oscillator, oscillating for 3 minutes violently, centrifuging for 5 minutes, and layering; sucking 6ml of supernatant, placing the supernatant into a dispersed solid phase extraction purification tube which is pre-filled with a purification material, vortexing to fully mix the supernatant, placing the supernatant on an oscillator to violently oscillate for 5 minutes to completely purify the supernatant, centrifuging the supernatant for 5 minutes, precisely sucking 2ml of supernatant, placing the supernatant on a nitrogen blowing instrument to concentrate the supernatant in a water bath at 40 ℃ until the supernatant is dry, precisely adding 0.2ml of 15% acetonitrile, vortexing the supernatant for 1 minute, performing ultrasonic treatment for 1 minute, mixing the supernatant evenly, centrifuging the mixture, and taking the supernatant to obtain the product;
s5, assay: precisely sucking 1 μ l of the matrix mixed reference solution and sample solution respectively, injecting into a liquid chromatogram-mass spectrometer, and measuring.
2. The method for detecting veterinary drug residues in bear gall powder according to claim 1, wherein the S5 liquid chromatography comprises a mobile phase, an elution mode and a selection instrument, and the mobile phase in the S5 liquid chromatography is any one of the following (1) to (4):
(1) mobile phase a 0.1% formic acid (containing 0.2mmol/L ammonium formate and 0.2mmol ammonium fluoride) solution-mobile phase B0.1% formic acid in acetonitrile;
(2) mobile phase a 0.2% formic acid (containing 0.3mmol/L ammonium formate and 0.3mmol ammonium fluoride) solution-mobile phase B0.1% formic acid in acetonitrile;
(3) mobile phase a 0.2% formic acid (containing 0.5mmol/L ammonium formate and 0.5mmol ammonium fluoride) solution-mobile phase B0.2% formic acid in acetonitrile;
(4) mobile phase a 0.1% formic acid (containing 0.4mmol/L ammonium formate and 0.4mmol ammonium fluoride) solution-mobile phase B0.2% formic acid in acetonitrile.
S5, adopting gradient elution in the liquid chromatography, wherein the flow of the gradient elution is any one of the following (1) to (3):
(1) 0-1.5 min, 1% of mobile phase B by volume percentage, 1.5-2.0 min, 1-10% of mobile phase B by volume percentage, 2.0-4.5 min, 10-18% of mobile phase B by volume percentage, 4.5-6 min, 18-22% of mobile phase B by volume percentage, 6-9 min, 22-30% of mobile phase B by volume percentage, 9-12 min and 30-35% of mobile phase B by volume percentage; 12-20 min, 35-80% of mobile phase B by volume percentage, 20-26 min, 80-100% of mobile phase B by volume percentage;
(2) 0-0.5 min, 2% of mobile phase B by volume percentage, 0.5-1.8 min, 2-15% of mobile phase B by volume percentage, 1.8-3.5 min, 10-15% of mobile phase B by volume percentage, 3.5-6 min, 15-25% of mobile phase B by volume percentage, 6-7 min, 25-30% of mobile phase B by volume percentage, 7-11 min and 30-35% of mobile phase B by volume percentage; 11-16 min, 35-100% of mobile phase B by volume percentage concentration, 16-26 min and 100% of mobile phase B by volume percentage concentration;
(3) 0-1.0 min, 3% of mobile phase B by volume percentage, 0.5-1.8 min, 2-15% of mobile phase B by volume percentage, 1.8-5 min, 10-15% of mobile phase B by volume percentage, 5-10 min, 15-20% of mobile phase B by volume percentage, 10-15 min, 20-30% of mobile phase B by volume percentage, 15-20 min and 30-35% of mobile phase B by volume percentage; 20-30 min, 35-100% of mobile phase B by volume percentage concentration, 30-35 min and 100% of mobile phase B by volume percentage concentration.
In the S5, in the mass spectrometry condition, the instrument adopts a triple quadrupole mass spectrometer, and Multiple Reaction Monitoring (MRM) is performed in an electrospray ionization (ESI) mode.
3. The method for detecting veterinary drug residues in bear gall powder according to claim 1, wherein the S4, 0.1mol/L Na2EDTA-McIlvaine buffer solution (pH4.0) is prepared by the following steps: 2.9g of citric acid monohydrate, 10.9g of disodium hydrogen phosphate dodecahydrate and 37.2g of disodium ethylene diamine tetraacetate dihydrate were weighed, water was added to 900ml, pH was adjusted to 4.0 with 1mol/L of sodium hydroxide solution, and volume was determined to 1L with water.
4. The method for detecting veterinary drug residues in bear gall powder as claimed in claim 1, wherein the S4 purifying material is magnesium sulfate 300mg, octadecylsilane chemically bonded silica 300mg, and N-Propylethylenediamine (PSA)1800 mg.
5. The method for detecting veterinary drug residues in bear gall powder as claimed in claim 1, wherein the vibration frequency of the vigorous shaking of S4 is 500 times/min.
6. The method for detecting veterinary drug residues in bear gall powder as claimed in claim 1, wherein the ratio of anhydrous sodium chloride to sodium sulfate added in S4 is 1: 4.
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