CN109596730B - Method for simultaneously determining hormone and antibiotic in fat food sample - Google Patents
Method for simultaneously determining hormone and antibiotic in fat food sample Download PDFInfo
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Abstract
The invention relates to the technical field of complex matrix extraction technology and medicine component detection, relates to a method for simultaneously determining hormone and antibiotic in fatty food, and particularly relates to a method for simultaneously determining hormone and antibiotic compounds in complex matrices such as pork. The invention uses a freeze dryer to freeze and dry a sample and then grinds the sample into powder, and then uses a rapid solvent extraction instrument and uses a mixed solvent of normal hexane, methanol and acetonitrile as an extracting agent to extract the sample. The volume ratio of the normal hexane to the methanol to the acetonitrile is as follows: 1:1-2:1: 2. The method can simultaneously extract a plurality of hormones and a plurality of antibiotics in the complex matrixes such as pork, and the extraction efficiency is obviously superior to that of other extraction methods.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of complex matrix extraction technology and medicine component detection, relates to a method for simultaneously determining hormone and antibiotic in a fat food sample, and particularly relates to a method for simultaneously determining hormone and antibiotic compounds in complex matrixes such as pork.
[ background of the invention ]
The rapid solvent extraction (ASE) technology is a method for efficiently and rapidly extracting organic matters in a solid or semisolid sample by using an organic or polar solvent at a high temperature (the temperature range is 50-200 ℃) and a pressure (7-12 Mpa) by using a rapid solvent extractor according to the principle that solutes have different solubilities in different solvents. The rapid solvent extraction is the latest extraction separation method which integrates short extraction time, less solvent consumption, less environmental pollution and automatic control.
Steroid hormones can be produced by the human body, playing a key role in physiology and having important effects. Steroid hormones are important drugs for anti-inflammatory, antipyretic and immunosuppressive purposes. It is also known as a growth inhibitor. Antibiotics refer to chemical substances produced by microorganisms (including bacteria, fungi and actinomycetes) or higher animals and plants in the life process, and the chemical substances have the effects of resisting pathogens or other active secondary metabolites and interfere with the development function of other living cells.
Steroid hormones have potentially negative effects on hormonal functions in humans and other animals, such as fertility decline, growth and development, and animal hermaphroditism and feminization. Many antibiotics are illegally abused in feeding pigs and other farm-raised animals, such as sheep and cattle. Steroid hormones and antibiotics are banned as growth promoters in european countries and china due to their detrimental effects on human health, such as food poisoning and potential hazards associated with residues in edible tissues and their products (e.g. ham sausages). The determination of steroid hormones and antibiotics in food products has become a matter of concern to researchers.
[ summary of the invention ]
The invention aims to provide a method for extracting steroid hormones and antibiotics in complex matrixes such as meat and the like by utilizing a rapid solvent extraction technology aiming at the problems in the prior art, and the method can effectively improve the extraction efficiency of the steroid hormones and the antibiotics and solve the problems of drug loss and the like in the experimental process caused by the complex matrixes. And solves the problems that the prior matrix is complex and influences the extraction effect, the efficiency is low, and the like.
The technical scheme of the invention is as follows:
a method for extracting hormone and antibiotic from fatty food sample comprises freeze drying the sample with a freeze dryer, grinding into powder, and extracting with a rapid solvent extraction instrument using mixed solvent of n-hexane, methanol and acetonitrile as extractant. The volume ratio of the normal hexane to the methanol to the acetonitrile is as follows: 1:1 to 2:1:2, preferably: 2: 1.
The fat food sample can be pork, beef and other fat-containing food;
the hormone is Dexamethasone (DX), chlormadinone acetate (CMA), medroxyprogesterone acetate (MPA), Allylpregnenol (ALO) benzene, nandrolone propionate (NPP) and Estradiol Benzoate (EB);
the antibiotic is Roxithromycin (RM), Sulfadimidine (SMR), Sulfadiazine (SD) and Enrofloxacin (EN);
specifically, the invention adopts the following technical scheme:
1) extracting fat food sample powder by using a rapid solvent extraction method (ASE), and collecting an extract of a combined solvent of n-hexane, methanol and acetonitrile;
2) determining the content of hormone and antibiotic in the extract liquid in the step 1) by adopting an LC-ESI-MS/MS method;
the fat food sample is a complex substrate such as pork;
the step 1) comprises the following substeps:
step S1: freeze-drying complex matrix such as pork, and pulverizing into powder with pulverizer;
step S2: sieving the pulverized powder, and uniformly mixing with diatomite;
step S3: placing the mixture obtained in the step S2 in an ASE extraction pool with a filter membrane, and adding sea sand until the sea sand is parallel to the pool mouth;
step S4: using n-hexane: methanol: extracting with a mixed solvent of acetonitrile, performing rotary drying by using a rotary evaporator after the extraction is finished, and performing extraction with methanol: acetonitrile: redissolving the mixed solvent of water, centrifuging and taking supernatant.
Preferably, the first and second electrodes are formed of a metal,
in step S2, the powder is sieved by a 40-100 mesh sieve;
the weight ratio of the powder to the diatomite is as follows: 1:1-1:3;
the volume of the ASE extraction pool in the step S3 is 30-40 ml;
in step S4, the ASE extraction conditions are as follows: the pressure is 1000-1500psi, the temperature is 40-100 ℃, the time is 5-15min, the cycle time is 1-3 times, the flushing volume is 80-150%, and the purging time is 100-300S;
in the S4, the centrifugation speed is 3000-4000r/min, and the centrifugation time is 5-10 min;
in the S4, the ratio of methanol: acetonitrile: the proportion of water is as follows: 1:1-2:1:2
In the step 2, the step of the method is carried out,
the detection parameters of the LC-ESI-MS/MS method are as follows:
ESI ion source; interface voltage is 3500-4000V; scanning positive ions; an MRM monitoring mode; the flow rate of the atomized gas is 2-3L/min, the flow rate of the drying gas is 8-10L/min, and the two gases are nitrogen; heating gas flow is 10-15L/min, and the gas is air; interface temperature is 280-300 ℃; the temperature of the desolventizing tube is 200-250 ℃; the temperature of the heating module is 300-400 ℃; the pressure of the collision gas is 2.7 multiplied by 105Pa, and the gas is argon;
the column was ACQUITYTM UPLC BEH C18(1.7 μm,2.1 mm. times.50 mm); the column temperature is 30-40 ℃;
the flow rate is 0.1-0.3 ml/min;
the mobile phase is 0.1-0.2% formic acid in acetonitrile.
Compared with the traditional method, the method has the following advantages:
the ASE extraction principle is as follows: a: the temperature is improved, the stiffness of the solvent is reduced, the prevention of the solvent entering a sample matrix is reduced, the diffusion of the solvent entering the sample matrix is increased, the surface tension between the solvent and the sample matrix is reduced, and the capacity of the solvent for dissolving the object to be detected is increased; b; the boiling point of the extraction liquid increases with increasing pressure, so that the solvent remains in liquid state at high temperature and high pressure and the dissolving capacity of the liquid to the solute is far larger than that of the gas to the solute. The method can simultaneously extract a plurality of hormones and a plurality of antibiotics in the complex matrixes such as pork, and the extraction efficiency is obviously superior to that of other extraction methods.
[ description of the drawings ]
FIG. 1 is a bar graph of steroid hormone and antibiotic controls;
a：ALO；b：CMA；c：DX；d：EB；e：EN；f：MPA；g：NPP；h：RM；i：SD；j：SMR。
[ detailed description ] embodiments
The following claims are hereby incorporated into the detailed description of the invention, with the understanding that the present disclosure is to be considered as a full and non-limiting example, and any limited number of modifications may be made without departing from the scope of the invention.
Example 1
1. Instrument and reagent
1.1 Instrument:
ACQUITYTM UPLC system (Woltes, Milford, Mass.), electronic analytical balance, Zhongjia LC-400 low speed centrifuge, Taxing freeze dryer, ASE 350 accelerated solvent extractor (Daian China Co., Ltd.), kq5200 ultrasonic cleaner (Kunshan ultrasonic Instrument Co., Ltd.), rotary evaporator re-5203 (Shanghai Yalong Biochemical instruments Co., Ltd.)
Liquid chromatograph
1.2 reagent:
water: meets the first-grade water specified in GB/T6682.
Methanol: analyzing and purifying;
acetonitrile: analyzing and purifying;
n-hexane: analyzing and purifying;
diatomite: 2 mm;
2. method of producing a composite material
2.1 preparation of control solutions
Taking appropriate amount of hormone and antibiotic reference substance, precisely weighing, and adding methanol to obtain solution of 1mg/ml each.
2.2 preparation of test solutions
Weighing about 0.2g of the powder (sieved by a third sieve) by the method of pharmacopoeia of 2015 edition, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of methanol, weighing, heating and refluxing for 5 hours, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the product.
The method for preparing the sample by the rapid solvent extraction (ASE) method comprises the following steps: crushing a sample by a crusher, sieving the crushed sample by a fourth sieve, precisely weighing about 3g of the crushed sample, uniformly mixing the weighed sample and 3g of diatomite for later use, transferring the sample into a 30-40ml extraction pool in which an ASE filter membrane is placed in advance, adding a proper amount of sea sand into the extraction pool, slightly shaking the extraction pool to enable the sea sand to be on the same horizontal line with a pool port, and screwing an upper cover of the extraction pool. After extraction, the extract was transferred to a rotary evaporator for spin-drying. Then, methanol is added: acetonitrile: redissolving the mixed solution of water at the ratio of 1:1-2:1:2 to the constant volume of 8-10ml, centrifuging at 3000-4000r/min for 5-10min, taking the supernatant, and determining by LC-ESI-MS/MS.
2.3 examination of ASE extraction conditions
2.3.1 examination of extraction adsorbents
The adsorbent also has a large influence on ASE. In this study, acidic silica gel, silica gel and alumina (baked at 100-20 ℃ C. for 20-24 hours) were studied without the effect of the adsorbent on the results.
Uses hexane, methanol and acetonitrile (1: 1, v/v/v) as extractant, and under the condition of 40-100 ℃, each circulation time is 5-10 minutes, the static extraction time is 5-15 minutes, and the pressure is 1000-1500 psi. The total flushing volume is 80-150%, the purging time is 100-300s, and the nitrogen flow rate. The results show that each adsorbent reduces the recovery of the compounds EN, MPA, FMQ, SD, EB. Thus, no adsorbent was added in the present invention and the majority of lipids were successfully removed in step 2 of the present invention, so no further study was performed considering any other adsorbent.
Several polar solvents and combinations thereof were tested as extraction solvents to obtain higher recoveries.
Seven solvents of acetonitrile, methanol, acetone, ethyl acetate, methanol: acetonitrile (1: 1, v/v), acetonitrile: acetone (1: 1, v/v), methanol: acetone (1: 1, v/v) were tested, and n-hexane was added to the above seven extraction solvents at a ratio of 1:1 to obtain a final solvent. The conditions of the ASE used are as follows: the extraction temperature is 40-100 ℃, 1000-1500psi, the static extraction time is 5-15 minutes, the washing volume is 80-150% of the cell size, and 1-3 cycles are carried out. Finally, when acetonitrile/methanol (1: 1, v/v) was used as the extraction solvent and n-hexane was added thereto at a ratio of 1:1, the recovery of the compound was statistically higher. Therefore, the invention adopts the combined solvent of n-hexane, methanol and acetonitrile as the extraction solvent.
Further, different proportional relations of n-hexane, methanol and acetonitrile are adjusted for testing. Under the condition of different proportions, the extraction recovery rates are different, when the volume ratio of the normal hexane, the methanol and the acetonitrile is 1:1-2:1:2, the extraction recovery rate is higher and can reach 90-120%, and when the volume ratio of the normal hexane, the methanol and the acetonitrile is 2:1, the extraction recovery rate is highest and can reach 100-120%.
2.3.2 examination of extraction pH
The pH of the extraction solvent was examined and an extraction solvent having a pH of 4-10 was prepared by adding appropriate amounts of ammonia and formic acid to methanol-acetonitrile (1: 1, v/v). The results show that higher recovery of the compound is observed at pH 6-8. Therefore, methanol-acetonitrile (1: 1, v/v) was chosen as the extraction solvent, without addition of acid or base.
2.3.3 examination of extraction time
To evaluate the effect of extraction time on extraction efficiency, different extraction times (5-15 minutes) were used. The results show that when the static extraction time is increased from 5 minutes to 15 minutes, the recovery rate increases and then decreases, with an optimum value at 8-12 minutes. Therefore, a static extraction time of 8-12 minutes was chosen.
2.3.4 examination of extraction temperature
Since temperature has a great influence on the extraction efficiency, a series of experiments were carried out at different temperatures (40-100 ℃) to determine the optimum extraction temperature. The results show that the recovery of the analyte reaches a maximum at 50-70 ℃. Therefore, 50-70 ℃ was chosen as the extraction temperature.
2.3.5 examination of percent flush volume
The percentage flush refers to the amount of solvent flushed through the cell after the static heating step, measured as a percentage of the cell volume. Larger wash volumes allow more solvent to pass through the sample. In this experiment, the flush volume was set to 50% -150%. The results show that the extraction efficiency reaches the highest value when the flush volume is set to 90-110%.
2.4ASE Final extraction conditions: the pressure is 1000-1500psi, the temperature is 50-70 ℃, the time is 8-12min, the times are 1-3, the flushing volume is 90-110%, and the purging time is 100-300 s.
2.5 chromatographic conditions and System suitability test
a) The instrument comprises the following steps: ACQUITYTM UPLC System (Watts corporation, Milford, Mass.)
b) A chromatographic column: ACQUITYTM UPLC BEH C18(1.7 μm,2.1 mm. times.50 mm)
c) Column temperature: 30-40 deg.C
d) Flow rate: 1-3ml/min
e) Mobile phase: 0.1-0.2% formic acid in acetonitrile
The theoretical plate number of the filler which is octadecylsilane chemically bonded silica is not less than 3000 calculated according to hormone and antibiotic peaks.
2.5 assay method
Measuring by high performance liquid chromatography (general rule 0512)
Precisely sucking 5ul of the reference solution and 5ul of the test solution, respectively, injecting into a liquid chromatograph-mass spectrometer, and measuring.
2.6 Standard Limit requirements
The European Union suggests minimum risk levels of Roxithromycin (RM), Sulfadimidine (SMR), Sulfadiazine (SD) and Enrofloxacin (EN) of 100 μ g/kg, respectively. For Dexamethasone (DX), chlormadinone acetate (CMA), medroxyprogesterone acetate (MPA) and Altrenogest (ALO), the minimum residual limit in the food is 0.75 to 4 mug/kg. Food is prohibited from containing Adenophora tetraphyllum (NPP) and Estradiol Benzoate (EB).
2.7 calculation (internal standard method)
In the formula Ai- -Peak surface of substanceProduct of large quantities
AsPeak area of deuterated reagent
CiConcentration of substance in ug/kg
Attention is paid to
Before use, the bottom of the extraction tank should be disassembled and cleaned, otherwise pressure instability is easily caused
The filter paper at the bottom of the extraction tank is arranged in the sealing ring, otherwise the filter paper causes leakage
The tightness is moderate when the extraction tank is filled with samples, and too loose easily causes excessive extraction liquid
Checking whether the air pressure of the air bottle reaches 1MPa before starting up
After the use, the water-cooled extraction tank is cleaned, and the extraction tank is dried in time (easy to rust).
3. Results
3.1 Linear relationship
Linear response was evaluated by adding 100. mu.l of 0, 2, 4, 8, 16, 32, 64, 128 fold diluted mixed standard solution and 100. mu.l of 0.012mg/ml deuterium erythromycin internal standard to 3g of the blank substrate (pork), respectively. All samples were done in duplicate and then submitted to the PLE process for pretreatment prior to UPLC-MS/MS. Then, a calibration curve was constructed using [ peak area/internal standard peak area ] of the analyte, based on the analyte concentration, and the results are detailed in table 1.
TABLE 1 Linear profile of hormones and antibiotics in fatty foods
3.2 accuracy and precision
Using QC samples, four points of low, medium, high and quantitative lower limit were prepared, 6 replicates for each concentration, and three consecutive days were run. The data obtained were used to calculate the recovery and relative standard deviation, the results of which are shown in table 2.
TABLE 2 Intra-and diurnal recoveries and relative reproducibility standard deviations of analytes in fat food samples
3.3 chromatographic assay
FIG. 1 is a bar graph of steroid hormone and antibiotic controls.
4. Discussion of the related Art
4.1 selection of ASE extraction solvent
In the present invention, the solvent used in the rapid solvent extraction was examined, and methanol was refluxed for 5 hours in the Chinese pharmacopoeia. In the experiment, methanol, normal hexane, acetonitrile, acetone and ethyl acetate are selected as extraction solvents for solvent investigation, and the result shows that the recovery rate of hormones and antibiotics is highest after the normal hexane, the methanol and the acetonitrile are extracted at the ratio of 2:1 (V: V), so the normal hexane, the methanol and the acetonitrile are preferably selected at the ratio of 2:1 (V: V) as the extraction solvents.
4.2 optimization of ASE extraction conditions
The melting boiling point of the methanol is higher, the rapid solvent extraction principle is hereinafter referred to as an extraction principle to improve the temperature and reduce the stiffness of the solvent, reduce the resistance of the solvent entering a sample matrix, increase the diffusion of the solvent entering the sample matrix, reduce the surface tension between the solvent and the sample matrix, increase the capacity of the solvent for dissolving a substance to be detected, increase the boiling point of the extraction liquid along with the increase of the pressure, and further keep the dissolving capacity of the solvent to the solute of the liquid under high temperature and high pressure to be far greater than the dissolving capacity of the gas to the solute. The response surface design is selected to adopt 60 ℃, the extraction is carried out for 14min, the extraction is carried out for 2 times, the content of the extract is close to that of pharmacopeia, and more extraction time, temperature and times have no obvious influence on the result. Finally, the optimum extraction process combination is determined to be extraction temperature of 60 ℃, extraction time of 14min and extraction times of 2 times.
The above description is only exemplary of the invention, and any modification, equivalent replacement, and improvement made within the spirit and scope of the present invention should be considered within the scope of the present invention.
Claims (4)
1. A method for simultaneously determining hormones and antibiotics in a fat food sample, comprising the steps of:
extracting fat food sample powder by adopting a rapid solvent extraction method, and collecting an extract of a combined solvent of n-hexane, methanol and acetonitrile;
determining the content of hormone and antibiotic in the extract liquid in the step 1) by adopting an LC-ESI-MS/MS method;
the step 1) comprises the following specific steps:
step S1: freeze-drying pork, and then crushing the pork into powder by a crusher;
step S2: sieving the pulverized powder, and uniformly mixing with diatomite;
step S3: placing the mixture obtained in the step S2 in an ASE extraction pool with a filter membrane, and adding sea sand until the sea sand is parallel to the pool mouth;
step S4: extracting with mixed solvent of n-hexane, methanol and acetonitrile, spin-drying with rotary evaporator, re-dissolving with mixed solvent of methanol, acetonitrile and water, centrifuging, and collecting supernatant;
in step S2, the mass ratio of the powder to the diatomaceous earth is: 1:1-1:3;
in the S4, when the volume ratio of n-hexane, methanol and acetonitrile is 1:1:1-2:1:2;
in the step S4, ASE extraction conditions are as follows: the pressure is 1000-1500psi, the temperature is 50-70 ℃, the time is 8-12min, the times are 1-3, the flushing volume is 90-110%, and the purging time is 100-300 s;
the hormone is one or more of dexamethasone, chlormadinone acetate, medroxyprogesterone acetate, allyl pregnenol, nandoxolone phenylpropionate or estradiol benzoate; the antibiotic is one or more of roxithromycin, sulfadimidine, sulfadiazine or enrofloxacin;
detection conditions of step 2):
ESI ion source, interface voltage 3500-4000V, positive ion scanning, MRM monitoring mode, atomizing gas flow rate of 2-3L/min, drying gas flow rate of 8-10L/min, both atomizing gas and drying gas being nitrogen, heating gas flow rate of 10-15L/min, the gas being air, interface temperature of 280-300 ℃, desolventizing tube temperature of 200-250 ℃, heating module temperature of 300-400 ℃, collision gas pressure of 2.7X 105Pa, the gas being argon;
a) the instrument comprises the following steps: ACQUITYTM UPLC system
b) A chromatographic column: ACQUITYTM UPLC BEH C18 with a size of 1.7 μm,2.1 mm × 50mm
c) Column temperature: 30-40 deg.C
d) Flow rate: 1-3ml/min
e) Mobile phase: 0.1-0.2% formic acid in acetonitrile.
2. The method of claim 1,
the volume of the ASE extraction pool in the step S3 is 30-40 ml.
3. The method of claim 1,
in the S4, the centrifugation speed is 3000-4000r/min, and the centrifugation time is 5-10 min.
4. The method of claim 1,
in the S4, the volume ratio of methanol to acetonitrile to water is as follows: 2:1:1.
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