CN104535671B - The detection method of metalaxyl residue in a kind of Fructus Solani melongenae - Google Patents
The detection method of metalaxyl residue in a kind of Fructus Solani melongenae Download PDFInfo
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- CN104535671B CN104535671B CN201410725518.1A CN201410725518A CN104535671B CN 104535671 B CN104535671 B CN 104535671B CN 201410725518 A CN201410725518 A CN 201410725518A CN 104535671 B CN104535671 B CN 104535671B
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Abstract
The invention discloses the detection method of metalaxyl residue in a kind of Fructus Solani melongenae.Method includes following step: (1) sample treatment: the Fructus Solani melongenae after plucking is placed in disintegrating machine broken, obtains Fructus Solani melongenae slurry；(2) extract: weighing Fructus Solani melongenae slurry 20g in conical flask, add the ethyl acetate of 100mL and acetone mixture, mechanical shaking extraction 60 70min under conditions of temperature is 35 40 DEG C, sucking filtration obtains clear liquid, is concentrated near dry, and nitrogen is blown to do, and redissolves standby with 2mL acetonitrile；(3) pillar separates: wash HLB pillar by 5mL ethyl acetate, again with 5ml washing with acetone pillar, loading, with the acetonitrile that 10mL volume ratio is 1:2 and water mixed liquid drip washing pillar, finally with the acetonitrile eluting of 10ml, collect eluent, rotation is steamed to 1ml, nitrogen dries up, and uses acetonitrile to be settled to 2ml, to be detected；(4) detection: use HPLC to detect.
Description
Technical field
The present invention relates to the detection method of metalaxyl residue in a kind of Fructus Solani melongenae, belong to the Detection Technologies of Pesticide Residues field.
Background technology
Metalaxyl belongs to hypotoxicity antibacterial.Former medicine rat acute LD50 of passing through mouth is 669 mgs/kg, acute percutaneous LD50 > 3100 milliliter/kilogram.Eyes and skin are had slight stimulation, and to Fish low toxicity, Squaliobarbus ourriculus TLM is 100 mgs/kg (96h).Metalaxyl belong to phenylamide efficiently, low toxicity, low-residual, interior absorption sterilization pesticide.Inhale in it and penetration be very strong, after dispenser 30 minutes can in plant upper and lower Bidirectional Conduction, the protected and therapeutical effect to disease plant; and the drug effect duration is long; the main synthesis suppressing pathogenic bacteria mycelium internal protein so that it is malnutrition, it is impossible to normal growth and dead.To Pseudoperonospora cubensis, phytophthora pathogenic bacteria and maize ear rot microbial various crop downy mildew, the phytophthora root rot of gourd, fruit and vegetable class, the downy mildew of millet are effective.
It is complicated that the most conventional method extracts process operation, needs the detection method of metalaxyl residue in a kind of simple detection Fructus Solani melongenae.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that the detection method of metalaxyl residue in a kind of Fructus Solani melongenae.
The present invention is achieved through the following technical solutions:
The detection method of metalaxyl residue in a kind of Fructus Solani melongenae, including following step:
(1) sample treatment: the Fructus Solani melongenae after plucking is placed in disintegrating machine broken, obtains Fructus Solani melongenae slurry；
(2) extract: weighing Fructus Solani melongenae slurry 20g in conical flask, add the ethyl acetate of 100mL and acetone mixture, mechanical shaking extraction 60-70min under conditions of temperature is 35-40 DEG C, sucking filtration obtains clear liquid, is concentrated near dry, and nitrogen is blown to do, and redissolves standby with 2mL acetonitrile；
(3) pillar separates: wash HLB pillar by 5mL ethyl acetate, again with 5ml washing with acetone pillar, loading, with the acetonitrile that 10mL volume ratio is 1:2 and water mixed liquid drip washing pillar, finally with the acetonitrile eluting of 10ml, collect eluent, rotation is steamed to 1ml, nitrogen dries up, and uses acetonitrile to be settled to 2ml, to be detected；
(4) detection: use HPLC to detect, testing conditions is: use C18 post, specification is 4.6*250mm, detection wavelength is 212nm, flowing mutually use acetonitrile and 0.5% aqueous acetic acid carry out gradient elution, 0-5min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 9:1, and 5-10min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 7:3,10-20min: pure acetonitrile；Flow velocity is 1.0mL/min.
The detection method of metalaxyl residue in described a kind of Fructus Solani melongenae, adds activated carbon in conical flask during vibration in step (2).
The detection method of metalaxyl residue in described a kind of Fructus Solani melongenae, in step (2), in ethyl acetate and acetone mixture, the volume ratio of ethyl acetate and acetone is 1:2.
The detection method of metalaxyl residue in described a kind of Fructus Solani melongenae, during sucking filtration, adds kieselguhr in buchner funnel.
The detection method of metalaxyl residue in described a kind of Fructus Solani melongenae, the model of HLB pillar is 3cc/60mg, 30 μm.
The detection method of metalaxyl residue in described a kind of Fructus Solani melongenae, during detection, sample size is 10 μ L.
The making of standard curve: take metalaxyl mark product and be configured to 0.01mg/L, 0.02 mg/L, 0.05 mg/L, 0.1 mg/L, 0.2 mg/L, the titer of 0.5 six concentration of mg/L and 1mg/L, HPLC is used to detect, testing conditions is: use C18 post, specification is 4.6*250mm, detection wavelength is 212nm, flowing mutually use acetonitrile and 0.5% aqueous acetic acid carry out gradient elution, 0-5min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 9:1,5-10min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 7:3,10-20min: pure acetonitrile；Flow velocity is 1.0mL/min.The numerical value obtained and concentration are depicted as standard curve.
Determination of recovery rates: take blank Fructus Solani melongenae slurry samples 10g tri-parts and be respectively placed in conical flask, adds the titer 1mL of 0.01mg/L, 0.1 mg/L and 1mg/L, each parallel five blank samples respectively, detects, calculate the response rate after extraction, pillar separate.
The beneficial effect that the present invention is reached:
The detection method of the present invention is simple to operation, and ethyl acetate and acetone mixed solution extraction ratio are high, can be with mass detection sample, and appearance time is 6.5min；Being computed, in good linear relationship in the concentration range of 0.01 mg/L-1 mg/L, correlation coefficient is 0.993, and the average recovery rate of three concentration from low to high is respectively 94.05%, and RSD value is 11.52%；95.25%, RSD value is 10.67%；96.81%, RSD value is 10.16%.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.Following example are only used for clearly illustrating technical scheme, and can not limit the scope of the invention with this.
Embodiment 1
In the present embodiment, the detection method of metalaxyl residue in a kind of Fructus Solani melongenae, including following step:
(1) sample treatment: the Fructus Solani melongenae after plucking is placed in disintegrating machine broken, obtains Fructus Solani melongenae slurry；
(2) extract: weighing Fructus Solani melongenae slurry 20g in conical flask, add the ethyl acetate of 100mL and acetone mixture, mechanical shaking extraction 60min under conditions of temperature is 40 DEG C, sucking filtration obtains clear liquid, is concentrated near dry, and nitrogen is blown to do, and redissolves standby with 2mL acetonitrile；
(3) pillar separates: wash HLB pillar by 5mL ethyl acetate, again with 5ml washing with acetone pillar, loading, with the acetonitrile that 10mL volume ratio is 1:2 and water mixed liquid drip washing pillar, finally with the acetonitrile eluting of 10ml, collect eluent, rotation is steamed to 1ml, nitrogen dries up, and uses acetonitrile to be settled to 2ml, to be detected；
(4) detection: use HPLC to detect, testing conditions is: use C18 post, specification is 4.6*250mm, detection wavelength is 212nm, flowing mutually use acetonitrile and 0.5% aqueous acetic acid carry out gradient elution, 0-5min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 9:1, and 5-10min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 7:3,10-20min: pure acetonitrile；Flow velocity is 1.0mL/min.
Wherein, in step (2), in ethyl acetate and acetone mixture, the volume ratio of ethyl acetate and acetone is 1:2；During sucking filtration, buchner funnel adds kieselguhr；The model of HLB pillar is 3cc/60mg, 30 μm；During detection, sample size is 10 μ L.
Embodiment 2
In the present embodiment, the detection method of metalaxyl residue in a kind of Fructus Solani melongenae, including following step:
(1) sample treatment: the Fructus Solani melongenae after plucking is placed in disintegrating machine broken, obtains Fructus Solani melongenae slurry；
(2) extract: weighing Fructus Solani melongenae slurry 20g in conical flask, add the ethyl acetate of 100mL and acetone mixture, mechanical shaking extraction 60min under conditions of temperature is 35 DEG C, sucking filtration obtains clear liquid, is concentrated near dry, and nitrogen is blown to do, and redissolves standby with 2mL acetonitrile；
(3) pillar separates: wash HLB pillar by 5mL ethyl acetate, again with 5ml washing with acetone pillar, loading, with the acetonitrile that 10mL volume ratio is 1:2 and water mixed liquid drip washing pillar, finally with the acetonitrile eluting of 10ml, collect eluent, rotation is steamed to 1ml, nitrogen dries up, and uses acetonitrile to be settled to 2ml, to be detected；
(4) detection: use HPLC to detect, testing conditions is: use C18 post, specification is 4.6*250mm, detection wavelength is 212nm, flowing mutually use acetonitrile and 0.5% aqueous acetic acid carry out gradient elution, 0-5min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 9:1, and 5-10min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 7:3,10-20min: pure acetonitrile；Flow velocity is 1.0mL/min.
Wherein, step (2) adds in conical flask activated carbon during vibration；In step (2), in ethyl acetate and acetone mixture, the volume ratio of ethyl acetate and acetone is 1:2；The model of HLB pillar is 3cc/60mg, 30 μm.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, on the premise of without departing from the technology of the present invention principle; can also make some improvement and deformation, these improve and deformation also should be regarded as protection scope of the present invention.
Claims (6)
1. a detection method for metalaxyl residue in Fructus Solani melongenae, is characterized in that, including following step:
(1) sample treatment: the Fructus Solani melongenae after plucking is placed in disintegrating machine broken, obtains Fructus Solani melongenae slurry；
(2) extract: weighing Fructus Solani melongenae slurry 20g in conical flask, add the ethyl acetate of 100mL and acetone mixture, mechanical shaking extraction 60-70min under conditions of temperature is 35-40 DEG C, sucking filtration obtains clear liquid, is concentrated near dry, and nitrogen is blown to do, and redissolves standby with 2mL acetonitrile；
(3) pillar separates: wash HLB pillar by 5mL ethyl acetate, again with 5ml washing with acetone pillar, loading, with the acetonitrile that 10mL volume ratio is 1:2 and water mixed liquid drip washing pillar, finally with the acetonitrile eluting of 10ml, collect eluent, rotation is steamed to 1ml, nitrogen dries up, and uses acetonitrile to be settled to 2ml, to be detected；
(4) detection: use HPLC to detect, testing conditions is: use C18 post, specification is 4.6*250mm, detection wavelength is 212nm, flowing mutually use acetonitrile and 0.5% aqueous acetic acid carry out gradient elution, 0-5min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 9:1, and 5-10min: volume ratio is acetonitrile and the aqueous acetic acid of 0.5% of 7:3,10-20min: pure acetonitrile；Flow velocity is 1.0mL/min.
In a kind of Fructus Solani melongenae the most according to claim 1, the detection method of metalaxyl residue, is characterized in that, adds activated carbon in step (2) during vibration in conical flask.
In a kind of Fructus Solani melongenae the most according to claim 1, the detection method of metalaxyl residue, is characterized in that, in step (2), in ethyl acetate and acetone mixture, the volume ratio of ethyl acetate and acetone is 1:2.
In a kind of Fructus Solani melongenae the most according to claim 1, the detection method of metalaxyl residue, is characterized in that, during sucking filtration, adds kieselguhr in buchner funnel.
In a kind of Fructus Solani melongenae the most according to claim 1, the detection method of metalaxyl residue, is characterized in that, the model of HLB pillar is 3cc/60mg, 30 μm.
In a kind of Fructus Solani melongenae the most according to claim 1, the detection method of metalaxyl residue, is characterized in that, during detection, sample size is 10 μ L.
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Effective date of registration: 20221012 Address after: No. 5, Yuexi Qianzhu Road, Wuzhong District, Suzhou City, Suzhou City, Jiangsu Province 215104 Patentee after: SUZHOU ELECTRICAL APPLIANCE SCIENCE RESEARCH INSTITUTE Co.,Ltd. Address before: 215129 4 4 Lu Shan Road, hi tech Zone, Suzhou, Jiangsu. Patentee before: SUZHOU GUOHUAN ENVIRONMENT DETECTION Co.,Ltd. |