CN103439419A - Experimental method of determining extracting agent for oxytetracycline residue in earthworm - Google Patents
Experimental method of determining extracting agent for oxytetracycline residue in earthworm Download PDFInfo
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Abstract
The invention provides an experimental method of determining an extracting agent for an oxytetracycline residue in an earthworm. The method comprises the following steps: 1) grinding an earthworm sample and Na2SO4 to prepare tissue slurry and cleaning the tissue slurry with extracting agents to obtain extract liquid; 2) carrying out stirring, oscillation, ultrasonic extraction and low-temperature high-speed centrifugation and collecting supernatant; 3) allowing the supernatant to pass through a polytetrafluoroethylene filter membrane to remove impurities and determining the content of oxytetracycline by using high performance liquid chromatography; 4) respectively calculating standard-added recovery rates of oxytetracycline by a variety of the extracting agents; and 5) subjecting a determined extracting agent to primary extraction and secondary extraction and determining an optimal scheme through variance analysis. The invention has the following advantages: through experiments, it is determined that a mixed liquor of methanol and water in a volume ratio of 4: 1 is an optimal extracting agent for extraction of the oxytetracycline residue in the earthworm; the purpose of effective extraction can be completely achieved through one extraction with the optimal extracting agent at room temperature, and the extraction needs a short period of time and low cost, is simple and easy to implement, has high extraction efficiency and is easy to popularize and apply.
Description
Technical field
The invention belongs to the Environmental Analytical Chemistry field, be specifically related to the experimental technique of Determination of oxytetracycline residues digestion agent in a kind of definite earthworm.
Background technology
Terramycin belongs to a kind of of TCs, has ten dihydro aphthacene based structures, is a kind of broad-spectrum antibiotics produced by actinomyces, and gram-positive bacteria, Gram-negative bacteria, anaerobion etc. are all had to resistance.
China is that microbiotic is used big country, and wherein terramycin is one of microbiotic that turnout and use amount are higher.According to statistics, China in 2000 is 10,000 tons of terramycin output only, account for 65% of Gross World Product, referring to: Hu Guanjiu, Wang Bing, grandson become. 5 kinds of teracycline antibiotic residues [J] in the high effective liquid chromatography for measuring environmental water sample. environmental chemistry, 2007,26 (1), 106-107.Terramycin is mainly used in livestock and poultry breeding industry; yet up to the Determination of oxytetracycline residues of 90-95% in feces of livestock and poultry; referring to: Beconi-Barker M G; Hornish R E, et al. Ceftiofur hy drochloride:plasma and tissue distribution in swine following in tramuscular administration at various doses [J]. Veterinary Pharmacology; Therapeutics, 1996,19 (3), 192-199.Along with feces of livestock and poultry is used for agricultural land soil as cheap fertilizer, and then cause serious pollution to soil environment, as in China, the terramycin content that can detect in soil is up to 200mg/kg, referring to: Wang Ran, Liu Tiezheng, Wang Tian. microbiotic lapsing to and eco-toxicity [J] in environment. Acta Ecologica Sinica, 2006,26 (1): 265-269.
In recent years, because the pollution of terramycin in soil has caused safely bad impact to soil ecology, therefore for being grown in biology in the terramycin contaminated soil, it is absorbed to Accumulation Phenomenon having obtained studying widely and paying close attention to.Wherein, in biosome, the extraction of terramycin is the gordian technique of Accurate Determining oxytetracycline residues, has directly determined the accuracy of final mensuration terramycin content.Due to the biological species property of there are differences, therefore same digestion agent might not be applicable to the extraction to terramycin in all biological species.Therefore be necessary to select optimum digestion agent to be extracted for different biological species, and set up simply, leach extraction method accurately and effectively.In GB/T 5009.95-2003, utilize Na
2the EDTA-McIlvaine damping fluid carries out extraction and determination to the TCses such as terramycin in honey.Boonsaner and Hawker, referring to: Boonsaner M, Hawker D W. Accumulation of oxytetracycline and norfloxacin from saline soil by soybeans. Science of the Total Environment. 2010,408:1731-1737, utilize Na
2the EDTA-McIlvaine damping fluid extracts the terramycin in the soybean body, but the extracting concentration of damping fluid is not explained and illustrated.Blackawell etc., referring to: Blackwell P A, Lutzhoft H C H, Ma H P et al. Fast and robust simultaneous determination of three veterinary antibiotics in groundwater and surface water using a tandem solid-phase extraction with high-performance liquid chromatography-UV detection[J]. Journal of Chromatography A, 2004, 1045 (1-2), 111-117, research is found: under ultrasonic auxiliary extraction, use Na
2eDTA-McIlvaine damping fluid-methyl alcohol extracts the terramycin in soil as digestion agent, and recovery of standard addition can be up to 27-75%.Juhel-Gauguin etc. study discovery, referring to: Juhel-Gaugain M., McEvoy J. D. G., VanGinkel L. A. Measurements for certification of chlortetracycline reference materials within the European Union Standards, Measuraments and Testing programme[J] Analytical Chemistry, 2000, 368 (7), 656-663, as digestion agent, the terramycin in animal tissue is had to extraction effect preferably with edta buffer liquid-methyl alcohol, recovery of standard addition can reach more than 75%.The reports such as Hu Xiangang, referring to: Hu Xiangang, Luo Yi, Zhou Qixing, Xu Lin. in 2008. Solid Phase Extraction-high Performance Liquid Chromatography animal excretions, 13 kinds of antibiotic medicines are residual. analytical chemistry, 36(9): 1162-1166, it is relatively good that the acetonitrile of citrate buffer solution acidifying extracts in pig manure the TCs effect such as terramycin.Anne, referring to: Anne Marie Jacobsen, Bent Halling-S rensen, Flemming Ingerslev, Steen Honor é Hansen. Simultaneous extraction of tetracycline, macrolide and sulfonamide antibiotics from agricultural soils using pressurised liquid extraction, followed by solid-phase extraction and liquid chromatography – tandem mass spectrometry. Journal of Chromatography A, 2004, 1038:157-170, proposition utilizes methyl alcohol-oxalic acid (volume ratio 1:1) to carry out good lixiviate to the terramycin in soil.At present, set up the perfect extracting method to terramycin in livestock and poultry meat, employing be the 5% perchloric acid extraction proposed in GB (GB/T 5009.116-2003).Otherness due to biological species, might not be suitable for the extraction of terramycin in the geobiont earthworm for the digestion agent that in soil, ight soil, honey, vegetables, livestock and poultry meat, terramycin is extracted, yet up to the present yet there are no about utilizing which kind of digestion agent to extract the proper research report of terramycin in earthworm.
In the leaching process of terramycin, usually adopt repeatedly the summation of extract to measure wherein terramycin content, complex steps wastes time and energy and wastes consumptive material.Therefore be necessary on the basis of selecting the optimum extraction agent, do not affecting extraction efficiency and extracting under the prerequisite of stability, simplify extraction step, improve extraction rate, will lay the foundation for absorption accumulation and the ecological risk of Accurate Prediction terramycin in geobiont earthworm body.
Summary of the invention
The objective of the invention is for above-mentioned existing problems, the experimental technique of Determination of oxytetracycline residues digestion agent in a kind of definite earthworm is provided, by screening, be suitable for the extraction agent of Determination of oxytetracycline residues in earthworm and set up simple, economic, effective extracting method.
Technical scheme of the present invention:
The experimental technique of Determination of oxytetracycline residues digestion agent in a kind of definite earthworm comprises the following steps:
1) fresh earthworm sample is placed in to the porcelain mortar, adds anhydrous Na
2sO
4, grind and prepare serum of tissue under condition of nitrogen gas, shift the serum of tissue after grinding, repeatedly clean mortar to cleaning residue with digestion agent, collect whole cleaning fluids and add digestion agent to required volume, obtain leaching liquor, described digestion agent is the potential various digestion agents of tool;
2) above-mentioned leaching liquor is vibrated under 18-25 ℃, 200r/min condition 20min, ultrasonic extraction 20min under the 100W condition then carries out high speed centrifugation with refrigerated centrifuge and separates 25min under 2500rmp, 4 ℃ of conditions, collects supernatant;
3) above-mentioned supernatant is crossed to 0.45 μ m teflon membrane filter and removed impurity, adopt high-performance liquid chromatogram determination terramycin content;
4) calculate respectively the recovery of standard addition of various digestion agents to terramycin, the selective extraction rate is at the digestion agent more than 80%, on this basis, select the digestion agent that the poor repeatability opposite sex less, lixiviate more stable of same digestion agent to the terramycin extraction rate, thereby determine the applicable digestion agent of terramycin extraction comparison in earthworm;
5) adopt above-mentioned definite digestion agent, carry out respectively a lixiviate and secondary lixiviate, compare the otherness of its extracting effect by variance analysis, and further its lixiviate stability is detected, between a lixiviate and secondary lixiviate total amount, do not present on the basis of significant difference, select a lixiviate to carry out lixiviate to terramycin, thereby simplify extraction time, improve extraction efficiency.
The potential various digestion agents of described tool comprise the citric acid acidifying acetonitrile that pH is 4.7, the Na of 0.1 mol/L pH4.0 ± 0.05
2the methyl alcohol that the methyl alcohol that the perchloric acid that EDTA-McIlvaine, concentration are 5w%, volume ratio are 1:1 and the mixed liquor of citric acid, volume ratio are 1:1 and mixed liquor and the methyl alcohol of different volumes ratio and the mixed liquor of water of edta buffer liquid.
Described earthworm sample and anhydrous Na SO
4mass ratio be 3:1.
The amount ratio of described earthworm sample and leaching liquor is 1.50g/20mL.
The methyl alcohol that the digestion agent that is suitable for a lixiviate of Determination of oxytetracycline residues in earthworm that described experiment is determined is volume ratio 4:1 and the mixed liquor of water.
Compared with prior art the present invention has the following advantages:
The method is by the comparison to the potential several digestion agent extraction effects of tool, and the methyl alcohol that the discovery volume ratio is 4:1 and the mixed liquor of water, be the optimum extraction agent of extracting terramycin in earthworm; Adopt this optimum extraction agent at room temperature to extract the purpose that once can reach effective lixiviate fully, thus the expense of having saved extraction time and having brought because of consumptive materials such as reagent, and method is simple, easy to implement and extraction efficiency is high, is easy to apply.
Embodiment
Embodiment:
Determine the preliminary preparation of the experimental technique of Determination of oxytetracycline residues digestion agent in earthworm, comprise following items:
(1) preparation of digestion agent
The citric acid acidifying acetonitrile that the present invention selects the potential digestion agent of tool to comprise that pH is 4.7, the Na of 0.1 mol/L pH4.0 ± 0.05
2eDTA-McIlvaine(is hereinafter to be referred as edta buffer liquid), the mixed liquor of perchloric acid that concentration is 5w%, methyl alcohol that volume ratio is 1:1 and citric acid, methyl alcohol that volume ratio is 1:1 and mixed liquor and the volume ratio of edta buffer liquid be respectively the methyl alcohol of 2:1,3:1,4:1 and the mixed liquor of water, its compound method is as follows.
1) preparation of edta buffer liquid
By Na
2hPO
4, Na
2eDTA and citric acid are mixed with respectively the aqueous solution of 0.2,0. 4 and 0.2 mol/L, first by citric acid solution and Na
2hPO
4solution is mixed with the McIlvaine damping fluid for 8:5 by volume, then by McIlvaine damping fluid and Na
2eDTA solution mixes for 1:1 by volume, finally with 6mol/L HCl or 6mol/L NaOH, regulates pH to 4.0 ± 0.05, obtains the Na of 0.1 mol/L
2the EDTA-McIlvaine damping fluid.
The preparation of the citric acid acidifying acetonitrile that 2) pH is 4.7
Sodium citrate and citric acid are hybridly prepared into respectively to the solution of 0.1M with water, be then that 18.6:1.4 mixes two kinds of solution according to volume ratio, is mixed with citrate buffer solution, regulates acetonitrile pH with citrate buffer solution and 4.7 get final product.
3) configuration of the mixed liquor of methyl alcohol and citric acid
The citric acid solution of methyl alcohol and 0.1mol/L is mixed and gets final product according to volume ratio 1:1.
The compound method of other digestion agents is with reference to 3) get final product.
(2) preparation of terramycin typical curve
1) preparation of standard mother liquor: take terramycin standard items 0.5000g,, use as mother liquor in the brown volumetric flask of 100ml by methanol constant volume;
2) the quantitatively preparation of curve post liquid: prepare 2 groups of quantitative curve post liquid with methyl alcohol dilution mother liquor, one group is low concentration group, concentration is set and is respectively 0.1mg/L, 0.2 mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L; Another group, for the high concentration group, arranges concentration and is respectively 1 mg/L, 3mg/L, 9mg/L, 12mg/L, 16 mg/L.
(3) the sample contamination is processed
Select the earthworm sample that not polluted by terramycin, put it into milled processed in mortar, the sample that takes 1.50g is put into the brown PE bottle of 40ml, 3 parallel sample are set, add the terramycin mother liquor 0.5mL that concentration is 15 mg/kg to be contaminated, process it is mixed with whirlpool, the pollution concentration that makes terramycin in biological sample is 5mg/kg, and under room temperature sealing lucifuge condition, standing 6h preserves.
This embodiment determines the experimental technique of Determination of oxytetracycline residues leaching liquor in earthworm, comprises the following steps:
1) fresh earthworm sample 1.50g is placed in to the porcelain mortar, adds the 0.50g anhydrous Na
2sO
4, grind and prepare serum of tissue under condition of nitrogen gas, shift the serum of tissue after grinding, repeatedly clean mortar to cleaning residue with different digestion agents respectively, collect whole cleaning fluids and add digestion agent to required volume, obtain leaching liquor;
2) above-mentioned leaching liquor is vibrated under 18-25 ℃, 200r/min condition 20min, ultrasonic extraction 20min under the 100W condition then carries out high speed centrifugation with refrigerated centrifuge and separates 25min under 2500rmp, 4 ℃ of conditions, collects supernatant;
3) above-mentioned supernatant is crossed to 0.45 μ m teflon membrane filter and removed impurity, adopt high-performance liquid chromatogram determination terramycin content; Described liquid chromatogram measuring condition is: water generation (Waters) high performance liquid chromatograph (HPLC) (comprising: 1525 binary pump, 717 type automatic samplers, 2487 UV-detector), water generation C18 reverse-phase chromatographic column (5 μ m * 0.46 * 250 mm), sample size is 20 μ L, 30 ℃ of column temperatures, flow velocity is 1ml/min, mobile phase is acetonitrile/0.01mol/L oxalic acid (v/v=20:80), detect wavelength 355 nm, retention time is 5.230 min, detectability 0.01 mg/L, quantitative limit 0.05 mg/L;
4) calculate the recovery of standard addition of different digestion agents to terramycin, the selective extraction rate is at the digestion agent more than 80%, on this basis, select the digestion agent that the poor repeatability opposite sex less, lixiviate more stable of same digestion agent to the terramycin extraction rate, thereby determine the applicable digestion agent of terramycin extraction comparison in earthworm;
5) adopt the above-mentioned digestion agent optimized, carry out respectively a lixiviate and secondary lixiviate, compare the otherness of its extracting effect by variance analysis, and further its lixiviate stability is detected, between a lixiviate and secondary lixiviate total amount, do not present on the basis of significant difference, select a lixiviate to carry out lixiviate to terramycin, thereby simplify extraction time, improve extraction efficiency.
The experimental result of this embodiment:
1) the digestion agent screening that in earthworm, terramycin extracts
Under same amount and extraction time condition, the first terramycin in ultrasonic extraction earthworm after the vibration, the recovery of standard addition experimental result of different digestion agents is shown in Table 1.For methyl alcohol: water, along with methyl alcohol is mentioned the increase of ratio, recovery of standard addition has increase tendency gradually, but the trend of this increase is stable gradually when this ratio is increased to 4:1, the recovery of standard addition difference obtained while with volume ratio, being 3:1 not significantly (
p0.05), but the recovery of standard addition of the terramycin obtained with other digestion agents have significant difference (
p<0.05).In addition, extract terramycin in the earthworm body with edta buffer liquid, methyl alcohol-citric acid and 5% perchloric acid and all obtained effect preferably, according to average recovery of standard addition, different digestion agents to the extracting effect of terramycin in the earthworm body are: methanol-water (V:V=4:1) > methanol-water (V:V=3:1) > edta buffer liquid > methyl alcohol: water (V:V=2:1) > methyl alcohol-citric acid (V:V=1:1) > 5% perchloric acid, and citric acid acidifying acetonitrile, methyl alcohol: therefore and be not suitable for for the satholith mycin in the lixiviate earthworm edta buffer liquid (V:V=1:1) is less than 15% due to recovery of standard addition.
The recovery of standard addition that the different digestion agent of table 1 extracts terramycin in earthworm relatively
2) leach extraction method optimization and the selection of terramycin in earthworm
1) research basis on, 4 kinds of digestion agents that selection has fine extracting effect are methanol-water (V:V=4:1), edta buffer liquid, methyl alcohol: citric acid (V:V=1:1), 5% perchloric acid carry out lixiviate stability and suitable extracting times is inquired into, and testing result is as shown in table 2.According to recovery of standard addition, be no matter a lixiviate or secondary lixiviate all with methyl alcohol: the extraction rate of water (V:V=4:1) is the highest.Judge that according to relative standard deviation RSD (%) stability of its lixiviate is reappearance and the precision of lixiviate, result shows, perchloric acid for 5% and methyl alcohol: for citric acid (V:V=1:1), between the recovery of standard addition of a lixiviate and secondary lixiviate, do not exist the significance difference opposite sex (
p0.05), although and methyl alcohol during the secondary lixiviate: the average recovery of standard addition of water (V:V=4:1) is up to 99.31%, but the RSD value is up to 7.493, and methyl alcohol during a lixiviate: the RSD value of water (V:V=4:1) is 0.666, therefore consider the stability of extraction rate and lixiviate, determine and adopt methyl alcohol: the preferred plan of a lixiviate of water (V:V=4:1) for terramycin residual in earthworm is extracted, and, a lixiviate have advantages of property simple to operate, consuming time short, cost consumption is low.
The comparison of the different extracting times extracting effects of terramycin in table 2 pair earthworm
Claims (5)
1. the experimental technique of Determination of oxytetracycline residues digestion agent in a definite earthworm is characterized in that comprising the following steps:
1) fresh earthworm sample is placed in to the porcelain mortar, adds anhydrous Na
2sO
4, grind and prepare serum of tissue under condition of nitrogen gas, shift the serum of tissue after grinding, repeatedly clean mortar to cleaning residue with digestion agent, collect whole cleaning fluids and add digestion agent to required volume, obtain leaching liquor, described digestion agent is the potential various digestion agents of tool;
2) above-mentioned leaching liquor is vibrated under 18-25 ℃, 200r/min condition 20min, ultrasonic extraction 20min under the 100W condition then carries out high speed centrifugation with refrigerated centrifuge and separates 25min under 2500rmp, 4 ℃ of conditions, collects supernatant;
3) above-mentioned supernatant is crossed to 0.45 μ m teflon membrane filter and removed impurity, adopt high-performance liquid chromatogram determination terramycin content;
4) calculate respectively the recovery of standard addition of various digestion agents to terramycin, the selective extraction rate is at the digestion agent more than 80%, on this basis, select the digestion agent that the poor repeatability opposite sex less, lixiviate more stable of same digestion agent to the terramycin extraction rate, thereby determine the applicable digestion agent of terramycin extraction comparison in earthworm;
5) adopt above-mentioned definite digestion agent, carry out respectively a lixiviate and secondary lixiviate, compare the otherness of its extracting effect by variance analysis, and further its lixiviate stability is detected, between a lixiviate and secondary lixiviate total amount, do not present on the basis of significant difference, select a lixiviate to carry out lixiviate to terramycin, thereby simplify extraction time, improve extraction efficiency.
2. determine according to claim 1 the experimental technique of Determination of oxytetracycline residues digestion agent in earthworm, it is characterized in that: the potential various digestion agents of described tool comprise the citric acid acidifying acetonitrile that pH is 4.7, the Na of 0.1 mol/L pH4.0 ± 0.05
2the methyl alcohol that the methyl alcohol that the perchloric acid that EDTA-McIlvaine, concentration are 5w%, volume ratio are 1:1 and the mixed liquor of citric acid, volume ratio are 1:1 and mixed liquor and the methyl alcohol of different volumes ratio and the mixed liquor of water of edta buffer liquid.
3. determine according to claim 1 the experimental technique of Determination of oxytetracycline residues digestion agent in earthworm, it is characterized in that: described earthworm sample and anhydrous Na SO
4mass ratio be 3:1.
4. determine according to claim 1 the experimental technique of Determination of oxytetracycline residues digestion agent in earthworm, it is characterized in that: the amount ratio of described earthworm sample and leaching liquor is 1.50g/20mL.
5. determine according to claim 1 the experimental technique of Determination of oxytetracycline residues digestion agent in earthworm, it is characterized in that: the digestion agent that is suitable for a lixiviate of Determination of oxytetracycline residues in earthworm that described experiment is determined is the volume ratio methyl alcohol that is 4:1 and the mixed liquor of water.
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