CN109580818B - Method for detecting florfenicol drug residue in pig hair - Google Patents
Method for detecting florfenicol drug residue in pig hair Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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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
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
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- G01N30/7266—Nebulising, aerosol formation or ionisation by electric field, e.g. electrospray
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention discloses a method for detecting florfenicol residual quantity in pig hair, which comprises the following steps: (1) pretreatment of a pig hair sample: cleaning, alkaline hydrolysis and organic solvent extraction; (2) the florfenicol-D3 standard working solution is used as an internal standard, and the florfenicol residual quantity in the pig hair is detected by ultra-high performance liquid chromatography-electrospray tandem mass spectrometry. The invention does not need to slaughter live pigs and other animals, realizes the detection of the living bodies of the animals, can accurately monitor whether the florfenicol is used in the growth process of the livestock and the poultry because the hair growth period is long and the drug metabolism is slow, has simple and convenient operation of the detection steps and has accurate and reliable detection results.
Description
Technical Field
The invention belongs to the field of drug residue detection, and particularly relates to a method for qualitatively and quantitatively detecting florfenicol drug residue in pig hair.
Background
Florfenicol, also known as florfenicol, is a fluorinated derivative of chloramphenicol, has no nitro group which is potentially caused by aplastic anemia in a molecular structure, and has wide antibacterial spectrum and easy absorption. Therefore, florfenicol has become a main substitute drug for chloramphenicol, and is widely used for the treatment of gram-positive bacteria, gram-negative bacteria and chloramphenicol-resistant bacteria in animals. However, the result of the reproductive toxicity test shows that florfenicol has the effects of blood toxicity, embryo toxicity and immunosuppression, and adverse reactions such as anorexia, diarrhea and the like can also occur after the florfenicol is taken, and the health of human bodies is greatly harmed by eating a large amount of pork with overproof florfenicol. Currently, because veterinary drugs are not used clinically, the florfenicol resistance of bacteria is also getting stronger and stronger, and multiple drug resistance is presented with the time. For a long time, the drug resistance of bacteria can be greatly improved, and common drugs have no effective inhibition effect on the bacteria. Not only does this result in economic waste, but it also increases the difficulty of veterinary clinical treatment, and even threatens human life safety.
Drug residue monitoring typically detects urine or blood samples from live animals, or tissue samples, such as muscle, liver, etc., from slaughtered animals. Due to the time lag of veterinary drug residue detection, and the action of biological macromolecules such as enzymes in biological tissues of veterinary drugs, the veterinary drugs are usually easy to metabolize and have high clearance, so that sometimes, the tracing of some abnormal or illegal veterinary drugs becomes difficult. Establishing a rapid and sensitive detection method and searching a biopsy material capable of being sampled in vivo are two important directions for veterinary drug residue analysis and research. In the past decade, the detection of illicit drugs such as stimulants in human hair by forensic medicine has been inspired, and the feasibility of animal hair as a test material has been studied and studied. Because animal hair is easy to collect, transport and store, and more importantly, the characteristic of safety evaluation can be made before slaughter, the hair lacks blood circulation, lacks various active substances for degrading drugs and has a quick excretion way, so that the drug metabolism is slow, and the retention time in the hair is far longer than that of other tissues. Compared with the common tissue samples (muscle, liver, kidney, fat, lung and the like), the hair can be obtained without slaughtering the animal, and is simple and convenient compared with the former. In addition, due to the structural and component characteristics of the hair and lower metabolic activity, the long retention time of the medicine in the hair after entering the hair is determined, and the medicine can be used as a long-term detection sample, which is incomparable to urine or blood, especially for the medicine with short half-life period, such as florfenicol and the like, after a certain period of medicine withdrawal, the medicine residue can not be detected from edible tissues or blood and urine to prove whether the forbidden medicine is used, and the hair can still be used as the detection sample for a longer period of time due to slow metabolism of the medicine in the hair, so that the proof of the forbidden medicine use is provided. Detecting whether the pig hair contains antiviral drug residues, thereby achieving the purpose of controlling the use of forbidden drugs from a breeding source. Therefore, the research and establishment of the method for detecting florfenicol drug residues in the pig hair have important significance for effectively monitoring the use of the drugs and ensuring the safety of animal food in China.
The method for detecting florfenicol residues in China has relatively few researches, and the national standard only comprises three items, namely liquid chromatogram-tandem mass spectrometry for determining the residual quantities of chloramphenicol, thiamphenicol and florfenicol in muscles, livers and aquatic products of edible animals GB/T20756-. Literature methods are Liquid Chromatography (LC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The methods are mainly applied to the determination of florfenicol medicaments in animal tissues, and the detection method of the florfenicol medicament residual quantity in pig hair is not reported.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a simple, convenient, rapid, sensitive, accurate and economic method for detecting the florfenicol drug residue in pig hair.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a method for detecting florfenicol residual quantity in pig hair is characterized by comprising the following steps: (1) pretreatment of a pig hair sample: cleaning, alkaline hydrolysis and organic solvent extraction; (2) the florfenicol-D3 standard working solution is used as an internal standard, and the florfenicol residual quantity in the pig hair is detected by an ultra-high performance liquid chromatography-electrospray tandem mass spectrometry method.
The pretreatment of the pig hair sample comprises the following steps:
a. cleaning: washing pig hair with tap water to remove visible impurities, ultrasonically treating the pig hair with 1% SDS for 15 minutes, washing with secondary water, and drying with filter paper; drying hair at 50 deg.C, and placing in a dryer for use;
b. hydrolysis: cutting into L-2mm with scissors, weighing hair 0.5g into 50mL polypropylene centrifugal tube, adding florfenicol-D3 standard working solution 50.0 μ L and 0.5mol/L sodium hydroxide solution 5mL, mixing, keeping temperature in 80 water C bath for 1 hr, taking out, and cooling to room temperature;
c. extraction: adding 10.0mL of acetonitrile, vortexing for 30s, performing ultrasonic extraction for 20min, adding 2g of sodium chloride, vortexing, mixing uniformly for 2min, centrifuging for 10min at 5000r/min, taking the supernatant in another tube, adding 10.0mL of acetonitrile, repeatedly extracting once, combining the supernatants, blowing nitrogen at 60 ℃ to dry, dissolving the residue with 1.00mL of water, vortexing for 30s, and filtering with a 0.22mm filter membrane.
The detection conditions of the ultra-high performance liquid chromatography-electrospray tandem mass spectrometry are as follows:
a. ultra-high performance liquid chromatography conditions: a chromatographic column: eclipse Plus C18(RRHD 1.8 μm, 2.1X 100 mm). The mobile phase A is 0.1 percent formic acid aqueous solution; b is acetonitrile. Gradient elution procedure: 0-1.0 min, 2% -10% B; 1.0-3.0 min, 10% -90% B; 3.0-3.1 min, 90-2% B; 3.1-5.0 min, and maintaining 2% of B. The flow rate is 0.25 mL/min; the column temperature is 30 ℃; sample introduction volume: 5.0 mu L;
b. electrospray tandem mass spectrometry conditions: ionization mode: electrospray ionization negative ion mode (ESI-); the detection mode is as follows: multiple Reaction Monitoring (MRM); capillary voltage: 4000V; ion source Temperature (TEM): 325 ℃; temperature of the drying gas: 300 ℃; flow rate of drying gas: 15L/min; atomizing gas pressure: 50 psi; temperature of sheath gas: 400 ℃; the flow rate of the sheath gas: 12L/min.
The residual amount of florfenicol in the sample is calculated as mass fraction X, the value is expressed in micrograms per kilogram (mu g/kg), and the single point correction is calculated according to the following formulas (1) and (2):
in the formula:
Ci-florfenicol concentration in the sample solution (μ g/L);
Cis-concentration of florfenicol-D3 internal standard in the sample solution (μ g/L);
Cs-florfenicol concentration in control solution (μ g/L);
c' is-concentration of florfenicol-D3 internal standard in control solution (. mu.g/L);
Ai-florfenicol peak area in the sample solution;
Ais-peak area of florfenicol-D3 internal standard in the sample solution;
As-florfenicol peak area in control solutions;
A′is-peak area of florfenicol-D3 internal standard in control solution;
x represents the residual quantity (mu g/kg) of florfenicol in the sample;
v is the final volume (mL) of the sample solution;
m-sample mass (g);
the standard curve calibration is calculated as equation (3):
Ci-florfenicol concentration (. mu.g/L) in the sample checked on the standard curve; (ii) a
V is the final volume (mL) of the sample solution;
m is the mass of the sample in grams (g).
Compared with the prior art, the invention has the following advantages:
1. the florfenicol drug residue in the pig hair is detected for the first time, and the method has higher recovery rate and lower detection limit and quantification limit.
2. When the blank pig hair addition concentration is 1.5, 10.0 and 50.0 mu g/kg, the average recovery rate of the florfenicol method is 83.2-107%, the relative standard deviation in the day is 3.54-6.08%, and the relative standard deviation in the day is 6.88-9.14%.
3. The florfenicol is quantified by an internal standard method, the detection Limit (LOD) of the florfenicol is 0.5 mu g/kg, and the quantification Limit (LOQ) is 1.5 mu g/kg.
To further illustrate the features and effects of the present invention, the following description is further provided in conjunction with the accompanying drawings.
Drawings
FIG. 1 is a graph of ion chromatography (355.8>184.8) of blank pig hair with florfenicol (1.50. mu.g/kg) added thereto in accordance with an embodiment of the present invention.
FIG. 2 is a graph of ion chromatography (355.8>335.8) of blank pig hair with florfenicol (1.50. mu.g/kg) added thereto in accordance with an embodiment of the present invention.
Detailed Description
The invention is further described by the following detailed description in conjunction with the accompanying drawings. It should be understood that the method described in the examples is only for illustrating the present invention and not for limiting the present invention, and that simple modifications of the preparation method of the present invention based on the concept of the present invention are within the scope of the claimed invention.
1. Preparation of standard solution:
standard stock solutions: weighing a proper amount of florfenicol standard substance, preparing 1.0mg/mL standard stock solutions by using methanol respectively, and storing the stock solutions at the temperature of minus 18 ℃ in a dark place.
Standard intermediate solution: taking 1mL of the standard stock solution, diluting the stock solution with methanol to obtain a standard intermediate solution with the mass concentration of 10.0mg/L, and storing the intermediate solution at-18 ℃ in a dark place.
Standard working solution: taking 1mL of the standard intermediate solution, diluting with secondary water to obtain a standard working solution with a mass concentration of 1.0mg/L, and storing at-4 ℃ in a dark place.
florfenicol-D3 Standard working solution: weighing a proper amount of florfenicol-D3 standard substance, preparing 1.0mg/mL standard stock solution by using methanol, then diluting the standard stock solution into a standard intermediate solution with the mass concentration of 10.0mg/L by using methanol, diluting the standard intermediate solution into a standard working solution with the mass concentration of 200.0 mu g/L by using secondary water, and storing the standard working solution at the temperature of minus 4 ℃ in a dark place.
2. Recovery and precision
Taking a blank pig hair sample, adding florfenicol mixed standard solution into the blank pig hair sample to respectively obtain 1.5, 10.0 and 50.0 mu g/kg, then carrying out sample pretreatment and measurement according to the method, wherein each addition level is measured for 6 times, the intra-day precision is obtained by measuring 6 parallel samples under 3 standard addition levels in 1d, the inter-day precision is obtained by measuring 3 samples under 3 standard addition levels in 6d (measured for 1 time every day), and the result shows that when the florfenicol addition concentration is 1.5, 10.0 and 50.0 mu g/kg, the average recovery rate of the method is 83.2-107%, the intra-day relative standard deviation is 3.54-6.08% and the inter-day relative standard deviation is 6.88-9.14%. The precision and relative standard deviation are shown in table 1.
Table 1 florfenicol intra-and inter-day precision and relative standard deviation (n ═ 6) added to blank pig hair
3. Optimizing mass spectrum conditions:
respectively preparing 1.0mg/L florfenicol and florfenicol-D3 standard solution, directly entering an ion source without passing through a chromatographic column, and carrying out ESI (ion implantation system) treatment-And respectively optimizing the mass spectrum conditions in the modes. Performing first-order mass spectrogram full scanning, determining parent ions of each target compound, optimizing to obtain in-source fragmentation voltage, performing ion scanning on the selected parent ions under the condition of the selected in-source fragmentation voltage, selecting 1 pair of fragment ions with relatively strongest abundance as quantitative ions, and selecting 1 pair or 2 pairs of fragment ions with relatively strongest abundance as qualitative ions, and optimizing the collision energy of the sub-ions respectively. Finally, parameters such as the pressure of the atomizing gas, the temperature of the drying gas, the flow rate and the like are respectively carried out in an MRM modeAnd (6) optimizing. The optimized mass spectrum conditions are shown in table 2.
TABLE 2 Mass Spectrometry optimization conditions for florfenicol and florfenicol-D3 in MRM monitoring mode
Quantitative ions
4. Sample assay
Washing pig hair with tap water to remove visible impurities, ultrasonically treating the pig hair with 1% SDS for 15 minutes, washing with secondary water, and drying with filter paper; drying hair at 50 deg.C, and placing in a dryer for use; shearing into L-2mm with scissors, weighing 0.5g of hair, putting the hair into a 50mL polypropylene centrifuge tube, adding 50.0 muL of florfenicol-D3 standard working solution and 5mL of 0.5mol/L sodium hydroxide solution, uniformly mixing, keeping the temperature in a water bath at 80 ℃ for 1 hour, taking out, cooling to room temperature, adding 10.0mL of acetonitrile, whirling for 30s, ultrasonically extracting for 20min, adding 2g of sodium chloride, whirling, uniformly mixing for 2min, centrifuging for 10min at 5000r/min, taking supernatant into another tube, adding 10.0mL of acetonitrile, repeatedly extracting once, combining the dried supernatants at 60 ℃ under nitrogen, dissolving residues with 1.00mL of water, whirling for 30s, filtering through a 0.22mm filter membrane, and measuring on a machine.
Setting the conditions of the liquid chromatogram as follows:
a chromatographic column: eclipse Plus C18(RRHD 1.8 μm, 2.1X 100 mm). The mobile phase A is 0.1 percent formic acid aqueous solution; b is acetonitrile. Gradient elution procedure: 0-1.0 min, 2% -10% B; 1.0-3.0 min, 10% -90% B; 3.0-3.1 min, 90-2% B; 3.1-5.0 min, and maintaining 2% of B. The flow rate is 0.25 mL/min; the column temperature is 30 ℃; sample introduction volume: 5.0. mu.L.
Electrospray tandem mass spectrometry conditions: ionization mode: electrospray ionization negative ion mode (ESI-); the detection mode is as follows: multiple Reaction Monitoring (MRM); capillary voltage: 2000V; ion source Temperature (TEM): 325 ℃; temperature of the drying gas: 325 ℃; flow rate of drying gas: 5L/min; atomizing gas pressure: 35 psi; temperature of sheath gas: 350 ℃; the flow rate of the sheath gas: 11L/min.
The detection result is shown in the attached drawing of the specification.
Of course, those skilled in the art should realize that the above embodiments are provided for illustrative purposes only and are not intended to limit the present invention, and that changes and modifications to the above embodiments are within the scope of the following claims.
Claims (3)
1. A method for detecting florfenicol residual quantity in pig hair is characterized by comprising the following steps:
(1) pretreatment of a pig hair sample:
a. cleaning: washing pig hair with tap water to remove visible impurities, ultrasonically treating the pig hair with 1% SDS for 15 minutes, washing with secondary water, and drying with filter paper; drying hair at 50 deg.C, and placing in a dryer for use;
b. hydrolysis: cutting the hair into L-2mm pieces with scissors, weighing 0.5g of hair into a 50mL polypropylene centrifuge tube, adding 50.0 mu L of florfenicol-D3 standard working solution and 5mL of 0.5mol/L sodium hydroxide solution, uniformly mixing, preserving heat in a water bath at 80 ℃ for 1 hour, taking out, and cooling to room temperature;
c. extraction: adding 10.0mL of acetonitrile, performing vortex extraction for 30s, performing ultrasonic extraction for 20min, adding 2g of sodium chloride, performing vortex mixing for 2min, performing centrifugation for 10min at 5000r/min, taking the supernatant into another centrifuge tube, adding 10.0mL of acetonitrile, performing repeated extraction once, combining the supernatants, performing nitrogen blow-drying at 60 ℃, dissolving the residue with 1.00mL of water, performing vortex extraction for 30s, and filtering with a 0.22mm filter membrane;
(2) detecting by adopting an ultra-high performance liquid chromatography-electrospray tandem mass spectrometry method:
a. ultra-high performance liquid chromatography conditions: a chromatographic column: RRHD 1.8 μm, 2.1 × 100 mm; the mobile phase A is 0.1 percent formic acid aqueous solution; b is acetonitrile; gradient elution procedure: 0-1.0 min, 2% -10% B; 1.0-3.0 min, 10% -90% B; 3.0-3.1 min, 90-2% of B; maintaining 2% of B for 3.1-5.0 min; wherein, the flow rate is 0.25mL/min, the column temperature is 30 ℃, and the sample injection volume is as follows: 5.0 muL;
b. electrospray tandem mass spectrometry conditions: ionization mode: electrospray ionization negative ion mode; the detection mode is as follows: monitoring multiple reactions; capillary voltage: 2000V; ion source temperature: 325 ℃; temperature of the drying gas: 325 ℃; flow rate of drying gas: 5L/min; atomizing gas pressure: 35 psi; temperature of sheath gas: 350 ℃; the flow rate of the sheath gas: 11L/min.
2. The method for detecting the residual amount of florfenicol in pig hair according to claim 1, further comprising the steps of:
preparation of standard solution:
a. standard stock solutions: weighing a proper amount of florfenicol standard substance, preparing 1.0mg/mL standard stock solutions by using methanol respectively, and storing the stock solutions at the temperature of minus 18 ℃ in a dark place;
b. standard intermediate solution: taking 1mL of the standard stock solution, diluting the stock solution with methanol to obtain a standard intermediate solution with the mass concentration of 10.0mg/L, and storing the standard intermediate solution at the temperature of minus 18 ℃ in a dark place;
c. standard working solution: taking 1mL of the standard intermediate solution, diluting with secondary water to obtain a standard working solution with the mass concentration of 1.0mg/L, and storing at-4 ℃ in a dark place;
d. florfenicol-D3 Standard working solution: weighing a proper amount of florfenicol-D3 standard substance, preparing 1.0mg/mL standard stock solution by using methanol, then diluting the standard stock solution into a standard intermediate solution with the mass concentration of 10.0mg/L by using methanol, diluting the standard intermediate solution into a standard working solution with the mass concentration of 200.0 mug/L by using secondary water, and storing the standard working solution at the temperature of minus 4 ℃ in a dark place.
3. Use of a detection method according to claim 1 or 2 for detecting residual amount of florfenicol in pig hair, wherein the detection method is used for detecting animal hair.
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