CN105116063B - The multi-joint detection method of cephalosporins medicine residual in a kind of dairy product - Google Patents
The multi-joint detection method of cephalosporins medicine residual in a kind of dairy product Download PDFInfo
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Abstract
The invention belongs to the detection technique field of animal derived food drug residue, it is a kind of method that high performance liquid chromatograph measures cephalosporins medicine residual quantity in dairy product.Including sample preextraction, Specification Curve of Increasing, instrument detection and analysis step, described detection method is a kind of multi-joint detection method being carried out using high performance liquid chromatography, and the medicine simultaneously detecting includes cefoperazone, cefotaxime, ceftriaxone, cefalotin.The present invention is limited to respectively 0.26mg/Kg, 0.01mg/Kg, 0.10mg/Kg, 0.07mg/Kg to the detection of 4 kinds of cephalosporins medicines such as cefoperazone, cefotaxime, ceftriaxone, cefalotin；Well, the response rate is 90%～105% to add linear relationship in concentration range in 1mg/kg～50mg/kg；Batch interior relative standard deviation≤15% of this method, relative standard deviation≤20% between batch.The present invention has the advantages that analysis time is short, test limit is low, precision is high, multi-joint detection, significant for cephalosporins medicine residual quantity in accurate monitoring milk.
Description
Technical field
The invention belongs to the detection technique field of animal derived food drug residue, it is one kind high performance liquid chromatograph
The method measuring cephalosporins medicine residual quantity in dairy product.
Background technology
With the fast development of China's animal husbandry, veterinary drug is reducing poultry sickness rate and fatality rate, is promoting animal productiong, changes
Kind animal meat product quality and raising efficiency of feed utilization aspect serve obvious action, it has also become important of Modern Animal Husbandry
Support.Cephalosporinses (Cephalosporins) belong to beta-lactam antibiotic, have penicillin resistant enzyme, curative effect height, toxicity
Low, anaphylaxiss are few, has a broad antifungal spectrum the features such as, can effectively suppress growth and the breeding of antibacterial.In farming animals cultivation, cephalo
Class antibiotic is widely used in prevention and the treatment of mammitis of cow, the controlling of the bacterial diseases of animal urethra, gastrointestinal tract and respiratory tract etc.
Treat and prevent and treat.But in actual breeding process, lack of standardization due to using method, not only cause the resistance to of animal derived bacterium cause of disease
The property of medicine rises, and causes the vicious cycle of overdose, and leads to the accumulation of the drug residue in livestock products, causes food
Potential safety hazard, gives people class and brings the serious harms such as allergy, alteration of intestinal flora, drug resistance rising.Therefore, the Ministry of Agriculture is clear and definite
Regulation (No. 560 bulletins of the Ministry of Agriculture)：" the up-to-date antibacterials that cefoperazone et al. cures clinic control use are used for food animal,
Drug resistance problems, impact animal epidemic control, food safety and human health can be produced, nullified product authentication code, no
Obtain reproduction, operation and use." at present the detection being directed to single medicine mostly is to the detection method of cephalo-type residue of veterinary drug, no
Adapt to multiple cephalo-type veterinary drugs at present are monitored, therefore, set up a kind of accurate, stable multi-joint detection method for realization
The effective monitoring of such medicine is significant.
Chinese patent (CN200910085945.7) disclose a kind of detection cephalosporins medicine enzyme linked immunological kit and
Its application, is detected to cephalo-type residue of veterinary drug by euzymelinked immunosorbent assay (ELISA), can only judge residual quantity roughly by light absorption value, resists
Preparation step is loaded down with trivial details, detects limit for height, is difficult to detect as accurate quantification.
Content of the invention
For solving above-mentioned technical problem, the present invention provides cephalosporins residual in a kind of detection by quantitative dairy product
Multi-joint detection method, meets the multi-joint detection demand of the cephalosporins to herding clinical field disabling.The present invention is to cephalo
The detection of 4 kinds of cephalosporins medicines such as piperazine ketone, cefotaxime, ceftriaxone, cefalotin be limited to respectively 0.26mg/kg,
0.01mg/Kg、0.10mg/kg、0.07mg/Kg；Add linear relationship in concentration range in 1mg/kg～50mg/kg well, to return
Yield is 90%～105%；Batch interior relative standard deviation≤15% of this method, relative standard deviation≤20% between batch.
The technical scheme is that a kind of multi-joint detection method of cephalosporins in detection milk, pre- including sample
Extraction, Specification Curve of Increasing, instrument detection and analysis step, described detection method is that the one kind being carried out using high performance liquid chromatography is many
Connection detection method, the medicine simultaneously detecting includes cefoperazone, cefotaxime, ceftriaxone, cefalotin, specifically includes as follows
Step：
(1) sample preextraction：Weigh milk sample to be placed in centrifuge tube, add albumen scavenger, after ultrasonic Treatment from
The heart, in Aspirate supernatant to test tube, nitrogen dries up, and adds and redissolves with the isopyknic methanol of sample -0.1% formic acid solution, adds
Fat-removal agent removes fat, vibration, centrifugation, and after discarding normal hexane, liquid is transferred in brown bottle after organic membrane filtration,
Standby；
Preferably weigh milk sample to be placed in centrifuge tube, add acetonitrile, ultrasonic Treatment, 5000rpm is centrifuged 10min,
To test tube, nitrogen dries up Aspirate supernatant, adds and redissolves with sample equal-volume methanol -0.1% formic acid solution, adds normal hexane
Remove fat, vibration, 5000rpm is centrifuged 10min, discards normal hexane, is transferred in brown bottle after organic membrane filtration, standby
With；
(2) drafting of standard solution preparation and standard curve：Take standard working solution, carried out with methanol -0.1% formic acid solution
Different multiples dilute, and draw standard curve；
It is preferably and accurately weighs cefoperazone, cefotaxime, ceftriaxone, each 100mg of cefalotin standard substance respectively, use
Simultaneously constant volume is configured to single standard solution in 4 10mL brown volumetric flasks to the dissolving of methanol -0.1% formic acid, then draws suitable respectively
The single standard solution of amount is transferred to precise volume setting in 1 10mL brown volumetric flask, is configured to the hybrid standard that concentration is 1mg/mL
Product stock solution.Hybrid standard product solution is diluted by again with methanol -0.1% formic acid solution through suitable, is configured to concentration and is respectively
The hybrid standard product working solution of 0.001mg/mL, 0.005mg/mL, 0.010mg/mL, 0.020mg/mL, 0.050mg/mL, adopts
High performance liquid chromatograph is analyzed, and draws standard curve, calculates standard regressive method；
(3) step (1) gained sample is entered the detection of high performance liquid chromatograph device, by testing result and described standard curve pair
Ratio obtains testing concentration.
Optimum condition is using Agilent 1100 type high performance liquid chromatograph；Agilent (C18,4.6 250,5 μm of x)
ZORBAX Eclipse Plus reversed phase chromatographic column；Mobile phase is A- methanol, B-0.1% formic acid solution, A: B (volume ratio)=3: 7
～4: 6；Detection wavelength is 254nm；Flow velocity is 1ml/min；Column temperature is 35 DEG C；Sample size is 20 μ l.
Further, the ultrasonic processing method in described step (1) is batch (-type), ultrasonic Treatment 5 seconds, intermittently 5 seconds,
60 circulations.
Further, the albumen scavenger in described step (1) is acetonitrile, and sample liquid is 1: 3～1 with the volume ratio of acetonitrile
∶4.
Further, the fat-removal agent in described step (1) is normal hexane, and sample liquid is 2 with the volume ratio of normal hexane:
1～2.5: 1.
Further, described methanol -0.1% formic acid solution, the volume ratio of formic acid and 0.1% formic acid is 3: 7～4: 6.
Further, the organic filter membrane in described step (1) is that two steps filter, that is, first through 0.45 μm of organic membrane filtration,
Filtered solution is again through 0.22 μm of organic membrane filtration.Interfering material in sample can effectively be removed, shorten process time, improve efficiency.
Further, described sample is the pure dairy productss of liquid or milk powder product.
The testing process of the present invention is as follows：
(1) sample pretreatment
Weigh 5g milk sample, be accurate to 0.01g, sample is placed in centrifuge tube, add 15～20mL acetonitrile, ultrasound wave
Vibration, that is, ultrasonic 5 seconds, is spaced 5 seconds, 60 circulations, 5000rpm is centrifuged 10min, takes supernatant, in Aspirate supernatant to test tube,
Nitrogen dries up, and adds methanol -0.1% formic acid solution (V/V 3: 7～4: 6) to redissolve, adds 2～2.5mL normal hexane grease removal, shake
Swing, 5000rpm is centrifuged 10min, discards normal hexane, first after through 0.45 μm and the laggard high performance liquid chromatograph of 0.22 μm of membrane filtration
Analysis.
(2) testing conditions set
Condition is using Agilent 1100 type high performance liquid chromatograph；Agilent (C18,4.6 250,5 μm of x)
ZORBAX Eclipse Plus reversed phase chromatographic column；Mobile phase is A- methanol, B-0.1% formic acid solution, A: B (volume ratio)=3: 7
～4: 6；Detection wavelength is 254nm；Flow velocity is 1ml/min；Column temperature is 35 DEG C；Sample size is 20 μ l.
(3) Specification Curve of Increasing
Accurately weigh cefoperazone, cefotaxime, ceftriaxone, each 100mg of cefalotin standard substance respectively, with methanol-
Simultaneously constant volume is configured to single standard solution in 4 10mL brown volumetric flasks for 0.1% formic acid dissolving, then draws single in right amount marking respectively
Quasi- product solution is transferred to precise volume setting in 1 10mL brown volumetric flask, is configured to the hybrid standard product deposit that concentration is 1mg/mL
Solution.Hybrid standard product solution is diluted by again with methanol -0.1% formic acid solution through suitable, is configured to concentration and is respectively
The hybrid standard product working solution of 0.001mg/mL, 0.005mg/mL, 0.010mg/mL, 0.020mg/mL, 0.050mg/mL, adopts
High performance liquid chromatograph is analyzed, and draws standard curve, calculates standard regressive method.
(4) step 1 gained sample is detected through high performance liquid chromatograph device, by testing result and described standard curve contrast
Obtain determinand testing result.
(5) blank experiment
In addition to being not added with sample, all carry out by said determination condition and step.
(6) result measures
1. qualitative determination
Under same test condition, the retention time of target compound and target compound in standard working solution in test liquid
Retention time ratio, deviation is within ± 5%.
2. quantitative determine
Materials solution and corresponding standard working solution, make multiple spot calibration, by external standard method with peak area quantification.Standard solution
And the response value in sample solution all should instrument detection the range of linearity within.
3. result calculates and states
Calculate the residual quantity of cephalosporins in sample by formula (a)：
In formula：
The residual quantity of cephalosporins, mg/kg in X- sample；
The concentration of cephalosporins in C- sample solution, μ g/mL；
V- final sample liquid constant volume, mL；
F- extension rate；
M- sample size, g.
Note：Result of calculation need to deduct blank value.Measurement result is represented with the arithmetic mean of instantaneous value of parallel assay twice, retains three
Position significant digits.
4. method sensitivity, accuracy and precision
Sensitivity：The inspection to 4 kinds of cephalosporins medicines such as cefoperazone, cefotaxime, ceftriaxone, cefalotin for this method
Rising limit is respectively 0.26mg/Kg, 0.01mg/Kg, 0.10mg/Kg, 0.07mg/Kg.
Accuracy：To adding in concentration range in 1mg/kg～50mg/kg, the response rate is 90%～105% to this method.
Precision：Batch interior relative standard deviation≤15% of this method, relative standard deviation≤20% between batch.
Compared with the prior art, the invention has the advantages that：
1st, the present invention adopts the residual quantity of cephalosporins in Milk by HPLC, and mobile phase uses first
Alcohol and 0.1% formic acid solution, proportioning is 3: 7～4: 6, can will be completely separable for 4 kinds of medicines it is ensured that sensitivity, it is to avoid each other
Interference.
2nd, extracting solution uses acetonitrile, can effectively remove isolating protein and partial fat class interfering material；In sample extraction mistake
In journey, fat is gone using normal hexane, can effectively remove the interfering material such as fat in sample substrate.
3rd, priority of the present invention carries out loading pre-treatment with the mode of 0.45 μm and 0.22 μm membrane filtration, can effectively remove sample
Interfering material in product, shortens process time, improves efficiency.
4. this method has been filled up current cephalo-type detection method and has been limitation for single medicine, enriches many joint inspections
Survey method, so as to have more the suitability, is conducive to the effective monitoring of food safety.
Brief description
Fig. 1：The retention time of ceftriaxone；
Fig. 2：The retention time of cefotaxime；
Fig. 3：The retention time of cefoperazone；
Fig. 4：The retention time of cefalotin；
Fig. 5：The separation spectrogram of cephalosporins；
Fig. 6：Ceftriaxone canonical plotting；
Fig. 7：Cefotaxime canonical plotting；
Fig. 8：Cefoperazone canonical plotting；
Fig. 9：Cefalotin canonical plotting.
Specific embodiment
Describe the technology contents of the present invention below by embodiment in detail.It will be appreciated by those skilled in the art that following realities
Apply example to be used to scope of the present invention is carried out with the description of exemplary, the phase of each parameter of the present invention is summarized with this
To scope, therefore it can not be interpreted as one kind restriction to the present invention.
Dairy product is broadly divided into liquid and solid-state, and therefore, the present invention selects most representational liquid milk in milk
With milk powder as the embodiment verified.
Embodiment 1：
The present embodiment is the mensure of cephalosporins residual quantity in liquid milk, comprises the steps of：
(1) sample pretreatment
Measure liquid milk sample 5mL, be placed in 50mL centrifuge tube, addition 15mL acetonitrile, supersonic oscillations (ultrasonic 5 seconds,
Interval 5 seconds, 60 circulations), 5000rpm is centrifuged 10min, and in Aspirate supernatant to test tube, nitrogen dries up, and adds isopyknic first
Alcohol -0.1% formic acid solution (v/v, 3/7) redissolves, and adds 2ml normal hexane grease removal, vibration, 5000rpm is centrifuged 10min, just discards
Hexane, first after through 0.45 μm and the laggard efficient liquid phase chromatographic analysis of 0.22 μm of membrane filtration；
(2) testing conditions set
Experiment high-efficient liquid phase chromatogram condition used
Agilent 1100 type high performance liquid chromatograph
Agilent (C18,4.6 250,5 μm of x) ZORBAX Eclipse Plus reversed phase chromatographic column
Mobile phase：A- methanol, B-0.1% formic acid solution, A: B (volume ratio)=3: 7
Detection wavelength：254nm
Flow velocity：1ml/min
Column temperature：35℃
Sample size：20μl
(3) Specification Curve of Increasing
Accurately weigh cefoperazone, cefotaxime, ceftriaxone, each 100mg of cefalotin standard substance respectively, with methanol-
Simultaneously constant volume is configured to single standard solution in 4 10mL brown volumetric flasks for 0.1% formic acid dissolving, then draws single in right amount marking respectively
Quasi- product solution is transferred to precise volume setting in 1 10mL brown volumetric flask, is configured to the hybrid standard product deposit that concentration is 1mg/mL
Solution.Hybrid standard product solution is diluted by again with methanol -0.1% formic acid solution through suitable, is configured to concentration and is respectively
The hybrid standard product working solution of 0.001mg/mL, 0.005mg/mL, 0.010mg/mL, 0.020mg/mL, 0.050mg/mL, adopts
High performance liquid chromatograph is analyzed, and draws standard curve, calculates standard regressive method；
(4) step 1 gained sample is carried out high performance liquid chromatograph device detection, by testing result and described standard curve pair
Ratio obtains testing concentration.
(5) sample detection and result calculate
1. qualitative determination
Under same test condition, the retention time of target compound and target compound in standard working solution in test liquid
Retention time ratio, deviation is within ± 5%.
2. quantitative determine
Materials solution and corresponding standard working solution, by external standard method with peak area quantification.Standard solution and sample solution
Middle cefoperazone, cefotaxime, ceftriaxone, cefalotin response value all should instrument detection the range of linearity within.Mark
Quasi- solution and sample solution feature chromatogram are referring to Fig. 1.
3. blank experiment, quantitative determination, in addition to being not added with sample, is all carried out by said determination condition and step.
4. result calculates and states
With concentration as abscissa, peak area is vertical coordinate, draws standard curve, then sample peak is analyzed processing,
Can get the concentration of cephalosporins medicine in sample liquid to be measured, calculate the concentration of cephalosporins medicine according to the following formula：
In formula：
The residual quantity of cephalosporins, mg/kg in X- sample；
The concentration of cephalosporins in C- sample solution, μ g/mL；
V- final sample liquid constant volume, mL；
F- extension rate；
M- sample size, g.
Note：Result of calculation need to deduct blank value.Measurement result is represented with the arithmetic mean of instantaneous value of parallel assay twice, retains three
Position significant digits.
(6) result is as shown in table 1
The measurement result of cephalosporins medicine recovery of standard addition and precision in table 1 milk powder
Embodiment 2：
The present embodiment is the mensure of cephalosporins residual quantity in solid-state milk, comprises the steps of：
(1) sample pretreatment
Measure solid-state milk sample 1g, add pure water 4ml, be placed in after mixing in 50mL centrifuge tube, add 20mL acetonitrile, surpass
Sonication (ultrasonic 5 seconds, be spaced 5 seconds, 60 circulations), 5000rpm is centrifuged 10min, and in Aspirate supernatant to test tube, nitrogen blows
Dry, add methanol -0.1% formic acid solution (v/v, 4/6) to redissolve, add 2.5ml normal hexane grease removal, vibration, 5000rpm is centrifuged
10min, discards normal hexane, first after through 0.45 μm and the laggard efficient liquid phase chromatographic analysis of 0.22 μm of membrane filtration；
(2) testing conditions set
Experiment high-efficient liquid phase chromatogram condition used
Agilent 1100 type high performance liquid chromatograph
Agilent (C18,4.6 250,5 μm of x) ZORBAX Eclipse Plus reversed phase chromatographic column
Mobile phase：A- methanol, B-0.1% formic acid solution, A: B (volume ratio)=4: 6
Detection wavelength：254nm
Flow velocity：1ml/min
Column temperature：35℃
Sample size：20μl
(3) Specification Curve of Increasing and testing sample detection
Accurately weigh cefoperazone, cefotaxime, ceftriaxone, each 100mg of cefalotin standard substance respectively, with methanol-
Simultaneously constant volume is configured to single standard solution in 4 10mL brown volumetric flasks for 0.1% formic acid dissolving, then draws single in right amount marking respectively
Quasi- product solution is transferred to precise volume setting in 1 10mL brown volumetric flask, is configured to the hybrid standard product deposit that concentration is 1mg/mL
Solution.Hybrid standard product solution is diluted by again with methanol -0.1% formic acid solution through suitable, is configured to concentration and is respectively
The hybrid standard product working solution of 0.001mg/mL, 0.005mg/mL, 0.010mg/mL, 0.020mg/mL, 0.050mg/mL, adopts
High performance liquid chromatograph is analyzed, and draws standard curve, calculates standard regressive method；
(4) by step 1 sample carry out high performance liquid chromatograph device detection, by testing result and described standard curve pair
Ratio obtains testing concentration.
(5) sample detection and result calculate
1. qualitative determination
Under same test condition, the retention time of target compound and target compound in standard working solution in test liquid
Retention time ratio, deviation is within ± 5%.
2. quantitative determine
Materials solution and corresponding standard working solution, by external standard method with peak area quantification.Standard solution and sample solution
Middle cefoperazone, cefotaxime, ceftriaxone, cefalotin response value all should instrument detection the range of linearity within.Mark
Quasi- solution and sample solution feature chromatogram are referring to Fig. 1.
3. blank experiment, quantitative determination, in addition to being not added with sample, is all carried out by said determination condition and step.
4. result calculates and states
With concentration as abscissa, peak area is vertical coordinate, draws standard curve, then sample peak is analyzed processing,
Can get the concentration of cephalosporins medicine in sample liquid to be measured, calculate the concentration of cephalosporins medicine according to the following formula：
In formula：
The residual quantity of cephalosporins, mg/kg in X- sample；
The concentration of cephalosporins in C- sample solution, μ g/mL；
V- final sample liquid constant volume, mL；
F- extension rate；
M- sample size, g.
Note：Result of calculation need to deduct blank value.Measurement result is represented with the arithmetic mean of instantaneous value of parallel assay twice, retains three
Position significant digits.
(6) result is as shown in table 2
The measurement result of cephalosporins medicine recovery of standard addition and precision in table 2 milk
Claims (3)
1. the multi-joint detection method that in a kind of dairy product, cephalosporins medicine remains is it is characterised in that described method is examined simultaneously
The medicine surveyed includes cefoperazone, cefotaxime, ceftriaxone, cefalotin；The method comprises the following steps：
(1) sample preextraction：Weigh milk sample to be placed in centrifuge tube, add albumen scavenger, be centrifuged after ultrasonic Treatment, inhale
Take supernatant to test tube, nitrogen dries up, add and redissolve with the isopyknic methanol of sample -0.1% formic acid solution, add fat clear
Except agent removes fat, vibration, centrifugation, after discarding normal hexane, liquid is transferred in brown bottle after organic membrane filtration, standby；
(2) drafting of standard solution preparation and standard curve：Take standard working solution, carry out difference with methanol -0.1% formic acid solution
Multiple dilutions, draw standard curve；
(3) step (1) gained sample is entered the detection of high performance liquid chromatograph device, testing result and described standard curve are contrasted
To testing concentration；
The parameter of the high performance liquid chromatography in described step (2) is as follows：Using Agilent 1100 type high performance liquid chromatograph；
Agilent (250,5 μm of C18,4.6x) ZORBAX Eclipse Plus reversed phase chromatographic column；Mobile phase is A- methanol, B-0.1%
Formic acid solution, volume ratio A：B=3：7～4：6；Detection wavelength is 254nm；Flow velocity is 1ml/min；Column temperature is 35 DEG C；Sample size
For 20 μ l；
Ultrasonic processing method in described step (1) is batch (-type), ultrasonic Treatment 5 seconds, intermittently 5 seconds, 60 circulations；
Albumen scavenger in described step (1) is acetonitrile, and sample liquid is 1 with the volume ratio of acetonitrile：3～1：4；
Fat-removal agent in described step (1) is normal hexane, and sample liquid is 2 with the volume ratio of normal hexane：1～2.5：1；
Described methanol -0.1% formic acid solution, the volume ratio of formic acid and 0.1% formic acid is 3：7～4：6.
2. in dairy product as claimed in claim 1 cephalosporins medicine residual multi-joint detection method it is characterised in that：Described
Organic filter membrane in step (1) is that two steps filter, and that is, first through 0.45 μm of organic membrane filtration, filtered solution has machine filter through 0.22 μm again
Membrane filtration.
3. in dairy product as claimed in claim 1 cephalosporins medicine residual multi-joint detection method it is characterised in that：Described
Sample is the pure dairy productss of liquid or milk powder product.
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| CN106198487A (en) * | 2016-07-05 | 2016-12-07 | 佳木斯大学 | The surface enhanced Raman detection method of Penicillin in Milk medicine |
| CN106501405B (en) * | 2016-11-01 | 2019-04-19 | 中国检验检疫科学研究院 | Cephalosporins remain quick screening method in a kind of animal muscle tissue |
| CN106885854B (en) * | 2017-03-01 | 2019-09-24 | 北京出入境检验检疫局检验检疫技术中心 | The remaining method of Cephalosporins and its sample-pretreating method in a kind of detection pluck |
| CN107941951A (en) * | 2017-11-28 | 2018-04-20 | 安徽农业大学 | A kind of method of Quercetin in efficient detection dendrobium candidum |
| CN111141837A (en) * | 2018-11-06 | 2020-05-12 | 江西省农业科学院农产品质量安全与标准研究所 | Method for detecting residual quantity of cefquinome in vegetables |
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