CN104535670A - Method for detecting residual carbendazim in ripe oranges - Google Patents
Method for detecting residual carbendazim in ripe oranges Download PDFInfo
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- CN104535670A CN104535670A CN201410725218.3A CN201410725218A CN104535670A CN 104535670 A CN104535670 A CN 104535670A CN 201410725218 A CN201410725218 A CN 201410725218A CN 104535670 A CN104535670 A CN 104535670A
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Abstract
The invention discloses a method for detecting residual carbendazim in ripe oranges, which comprises the following steps: 1)dividing the ripe oranges into peels and pulp, cutting the oranges pulp, squeezing the oranges pulp to fruit juice for standby; 2)respectively taking the peels and orange pulp in a conical flask, adding a methanol aqueous solution and hydrochloric acid, performing ultrasonic extraction for 30-50 minutes; performing pumping filtration to obtain clear liquid, placing clear liquid in a separating funnel filled with sodium chloride, adding ethyl acetate and extracting twice, standing and layering, merging an upper level liquid, concentrating to lower than 5mL, metering volume to 5mL by ethyl acetate to obtain a sample liquid for standby; 3)using ethyl acetate for washing a C18 columella, sampling, using a methanol aqueous solution with volume ratio of 1: 1 for washing, using the methanol aqueous solution with volume ratio of 4: 1 for washing, finally using the methanol solution for eluting to obtain an eluate, metering volume of the eluate to 5mL by methanol, waiting for detecting; and 4)employing HPLC for detecting.
Description
Technical field
The present invention relates to the detection method that in a kind of ripe orange, carbendazim is residual, belong to the Detection Technologies of Pesticide Residues field.。
Background technology
Carbendazim belongs to benzimidazole, and english common name is carbendazim, and chemical name is benzimidazolyl-2 radicals-Ji chloro methyl formate, and its molecular formula is C9N3H10O2.Its sterling is white crystals, fusing point 310 DEG C (decomposition), and water-soluble hardly, solubleness is in organic solvent respectively acetone 300mg/l, chloroform 100mg/l, methylene chloride 68mg/l.Dissolve in diluted mineral acid and organic acid forms corresponding salt.
Carbendazim is a kind of low toxicity efficient germicide, belongs to low toxicity wide spectrum systemic fungicide by China's pesticide toxicity grading criteria.Its main mechanism is the formation of Spindle in the mitosis of interference bacterium, thus affect cell division, to many sac fungus and Fungi Imperfecti all effectively, and to oomycetes and bacterial disease invalid.Mainly all had good therapeutic effect to the sprout term disease of Pyricularia oryzae Cav, wheat, barley and highland barley head blight, sclerotinia rot of colza and cotton, vegetables etc., but since the eighties, pathogen is day by day serious to its resistance.In recent years, the new Pesticidal products derived by carbendazim and formulation agents constantly occur, and constantly for preventing and treating various disease, wherein, using carbendazim orgnic acid salts to prevent and treat various crop storage period disease fraud carbendazim and having better preventive effect.According to the regulation of FAO (Food and Agriculture Organization of the United Nation) (FAO), the residual quantity of carbendazim in fruits and vegetables should lower than 0.5mg/kg, the national regulations of China identical with the regulation of FAO (Food and Agriculture Organization of the United Nation) (GB18406.1-2001).
The assay method of Determination of carbendazim residue has a lot, as high efficiency liquid phase chromatographic analysis method, and infrared spectroscopy, vapor-phase chromatography, thin layer chromatography scanning, visible ray colourimetry and ultraviolet spectroscopy, fluorometry etc.But conventional extracting method complicated operation, and not for the special method of ripe orange, the amount that carbendazim remains in tangerine peel and pulp should be different, orange integrally can not be detected.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the detection method that in a kind of ripe orange, carbendazim is residual is provided.
The present invention is achieved through the following technical solutions:
The detection method that in ripe orange, carbendazim is residual, comprises following step:
(1) sample preparation: ripe orange is divided into tangerine peel and pulp two parts, tangerine peel shreds, and pulp juice extractor explodes into fruit juice, for subsequent use;
(2) extract: get tangerine peel 25g and pulp 50g is placed in conical flask respectively, add the methanol aqueous solution of 50mL and 100mL respectively, and add the hydrochloric acid of 0.1mL and 0.2mL respectively, ultrasonic extraction 30-50min; Obtain clear liquid after suction filtration, clear liquid is placed in the separating funnel being added with sodium chloride, add the ethyl acetate of 100mL and 200mL respectively, extracting twice, merges supernatant liquid after stratification, is concentrated into below 5mL, be settled to 5mL with ethyl acetate, obtain sample liquid for subsequent use;
(3) pillar is separated: with 10mL ethyl acetate washing C18 pillar, loading, with the methanol aqueous solution washing that 5mL volume ratio is 1:1, be the methanol aqueous solution washing of 4:1 again by 5mL volume ratio, finally use 10mL methanol solution wash-out, obtain eluent, eluent is concentrated into below 5mL, by methanol constant volume to 5mL, to be detected;
(4) detect: adopt HPLC to detect, testing conditions is: adopt C18 post, specification is 4.6*250mm, and determined wavelength is 280nm, and mobile phase adopts volume ratio to be the methyl alcohol of 9:1 and the aqueous acetic acid of 0.5%, and flow velocity is 1.0mL/min.
The detection method that in described a kind of ripe orange, carbendazim is residual, in step (2), in methanol aqueous solution, the volume ratio of methyl alcohol and water is 2:5.
The detection method that in described a kind of ripe orange, carbendazim is residual, described hydrochloric acid is the pure concentrated hydrochloric acid of common commercially available analysis.
The detection method that in described a kind of ripe orange, carbendazim is residual, in step (2), the sodium chloride added during extraction is 5-7g.
The detection method that in described a kind of ripe orange, carbendazim is residual, extracts after the clear liquid obtained by suction filtration is concentrated in step (2) again.
The detection method that in described a kind of ripe orange, carbendazim is residual, the specification of C18 pillar used is 500mg, 6mL.
The making of typical curve: get the titer that carbendazim mark product are mixed with 0.01mg/L, 0.02 mg/L, 0.05 mg/L, 0.1 mg/L, 0.2 mg/L, 0.5 mg/L and 1mg/L, six concentration, HPLC is adopted to detect, testing conditions is: determined wavelength is 280nm, mobile phase adopts volume ratio to be the methyl alcohol of 9:1 and the aqueous acetic acid of 0.5%, and flow velocity is 1.0mL/min.The numerical value obtained and concentration are depicted as typical curve.
Determination of recovery rates: get blank tangerine peel 25g and pulp 50g and be placed in conical flask respectively, add the titer 1mL of 0.5 mg/L respectively, through extracting, pillar detects after being separated, and parallelly makees five blank samples, calculates the recovery.
The beneficial effect that the present invention reaches:
Detection method of the present invention by tangerine peel and pulp separate detection, more rationally; With methyl alcohol and water mixed solution as extract, extraction effect is good, and ultrasonic extraction improves the efficiency of extraction; Carbendazim is transferred to ethyl acetate phase, C18 good separating effect by extraction, adopt HPLC to detect, appearance time is 3.8min, and lowest detection is limited to 0.01 mg/L, goes out peak quick; As calculated, in good linear relationship in the concentration range of 0.01 mg/L-1 mg/L, related coefficient is 0.995, and average recovery rate is 94.27%, RSD value is 9.92%.。
Embodiment
Below in conjunction with embodiment, the invention will be further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Embodiment 1
In the present embodiment, the detection method that in a kind of ripe orange, carbendazim is residual, comprises following step:
(1) sample preparation: ripe orange is divided into tangerine peel and pulp two parts, tangerine peel shreds, and pulp juice extractor explodes into fruit juice, for subsequent use;
(2) extract: get tangerine peel 25g and pulp 50g is placed in conical flask respectively, add the methanol aqueous solution of 50mL and 100mL respectively, and add the hydrochloric acid of 0.1mL and 0.2mL respectively, ultrasonic extraction 30-50min; Obtain clear liquid after suction filtration, clear liquid is placed in the separating funnel being added with sodium chloride, add the ethyl acetate of 100mL and 200mL respectively, extracting twice, merges supernatant liquid after stratification, is concentrated into below 5mL, be settled to 5mL with ethyl acetate, obtain sample liquid for subsequent use;
(3) pillar is separated: with 10mL ethyl acetate washing C18 pillar, loading, with the methanol aqueous solution washing that 5mL volume ratio is 1:1, be the methanol aqueous solution washing of 4:1 again by 5mL volume ratio, finally use 10mL methanol solution wash-out, obtain eluent, eluent is concentrated into below 5mL, by methanol constant volume to 5mL, to be detected;
(4) detect: adopt HPLC to detect, testing conditions is: adopt C18 post, specification is 4.6*250mm, and determined wavelength is 280nm, and mobile phase adopts volume ratio to be the methyl alcohol of 9:1 and the aqueous acetic acid of 0.5%, and flow velocity is 1.0mL/min.
Wherein, in step (2), in methanol aqueous solution, the volume ratio of methyl alcohol and water is 2:5, and described hydrochloric acid is the pure concentrated hydrochloric acid of common commercially available analysis.In step (2), the sodium chloride added during extraction is 5-7g.The specification of C18 pillar used is 500mg, 6mL.
Embodiment 2
In the present embodiment, the detection method that in a kind of ripe orange, carbendazim is residual, comprises following step:
(1) sample preparation: ripe orange is divided into tangerine peel and pulp two parts, tangerine peel shreds, and pulp juice extractor explodes into fruit juice, for subsequent use;
(2) extract: get tangerine peel 25g and pulp 50g is placed in conical flask respectively, add the methanol aqueous solution of 50mL and 100mL respectively, and add the hydrochloric acid of 0.1mL and 0.2mL respectively, ultrasonic extraction 30-50min; Obtain clear liquid after suction filtration, clear liquid is placed in the separating funnel being added with sodium chloride, add the ethyl acetate of 100mL and 200mL respectively, extracting twice, merges supernatant liquid after stratification, is concentrated into below 5mL, be settled to 5mL with ethyl acetate, obtain sample liquid for subsequent use;
(3) pillar is separated: with 10mL ethyl acetate washing C18 pillar, loading, with the methanol aqueous solution washing that 5mL volume ratio is 1:1, be the methanol aqueous solution washing of 4:1 again by 5mL volume ratio, finally use 10mL methanol solution wash-out, obtain eluent, eluent is concentrated into below 5mL, by methanol constant volume to 5mL, to be detected;
(4) detect: adopt HPLC to detect, testing conditions is: adopt C18 post, specification is 4.6*250mm, and determined wavelength is 280nm, and mobile phase adopts volume ratio to be the methyl alcohol of 9:1 and the aqueous acetic acid of 0.5%, and flow velocity is 1.0mL/min.
Wherein, in step (2), in methanol aqueous solution, the volume ratio of methyl alcohol and water is 2:5.Described hydrochloric acid is the pure concentrated hydrochloric acid of common commercially available analysis.In step (2), the sodium chloride added during extraction is 7g.Extract again after the clear liquid obtained by suction filtration in step (2) is concentrated.The specification of C18 pillar used is 500mg, 6mL.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and distortion, these improve and distortion also should be considered as protection scope of the present invention.
Claims (6)
1. the detection method that in ripe orange, carbendazim is residual, is characterized in that, comprise following step:
(1) sample preparation: ripe orange is divided into tangerine peel and pulp two parts, tangerine peel shreds, and pulp juice extractor explodes into fruit juice, for subsequent use;
(2) extract: get tangerine peel 25g and pulp 50g is placed in conical flask respectively, add the methanol aqueous solution of 50mL and 100mL respectively, and add the hydrochloric acid of 0.1mL and 0.2mL respectively, ultrasonic extraction 30-50min; Obtain clear liquid after suction filtration, clear liquid is placed in the separating funnel being added with sodium chloride, add the ethyl acetate of 100mL and 200mL respectively, extracting twice, merges supernatant liquid after stratification, is concentrated into below 5mL, be settled to 5mL with ethyl acetate, obtain sample liquid for subsequent use;
(3) pillar is separated: with 10mL ethyl acetate washing C18 pillar, loading, with the methanol aqueous solution washing that 5mL volume ratio is 1:1, be the methanol aqueous solution washing of 4:1 again by 5mL volume ratio, finally use 10mL methanol solution wash-out, obtain eluent, eluent is concentrated into below 5mL, by methanol constant volume to 5mL, to be detected;
(4) detect: adopt HPLC to detect, testing conditions is: adopt C18 post, specification is 4.6*250mm, and determined wavelength is 280nm, and mobile phase adopts volume ratio to be the methyl alcohol of 9:1 and the aqueous acetic acid of 0.5%, and flow velocity is 1.0mL/min.
2. the detection method that in a kind of ripe orange according to claim 1, carbendazim is residual, is characterized in that, in step (2), in methanol aqueous solution, the volume ratio of methyl alcohol and water is 2:5.
3. the detection method that in a kind of ripe orange according to claim 1, carbendazim is residual, it is characterized in that, described hydrochloric acid is the pure concentrated hydrochloric acid of common commercially available analysis.
4. the detection method that in a kind of ripe orange according to claim 1, carbendazim is residual, it is characterized in that, in step (2), the sodium chloride added during extraction is 5-7g.
5. the detection method that in a kind of ripe orange according to claim 1, carbendazim is residual, is characterized in that, extracts after the clear liquid obtained by suction filtration is concentrated in step (2) again.
6. the detection method that in a kind of ripe orange according to claim 1, carbendazim is residual, it is characterized in that, the specification of C18 pillar used is 500mg, 6mL.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699513A (en) * | 2016-01-21 | 2016-06-22 | 中华人民共和国赤峰出入境检验检疫局 | Method for detecting residues of carbendazol and thiabendazole in fruit and vegetable juice by high performance liquid chromatography |
| CN108572227A (en) * | 2018-06-22 | 2018-09-25 | 苏州仁益生物科技有限公司 | A kind of vegetables detection remaining method of carbendazim of agricultural |
| CN110186914A (en) * | 2018-08-08 | 2019-08-30 | 珠海市慧康生物科技有限公司 | A kind of fruit press and Fast Determination of Pesticide Residue all-in-one machine and detection method |
| CN112461808A (en) * | 2019-09-06 | 2021-03-09 | 苏州市农产品质量安全监测中心 | Detection method and kit for detecting carbendazim in agricultural products |
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2014
- 2014-12-04 CN CN201410725218.3A patent/CN104535670A/en active Pending
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| 刘双双 等: "多菌灵在稻田水、土壤及稻米中的残留研究", 《环境科学与管理》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699513A (en) * | 2016-01-21 | 2016-06-22 | 中华人民共和国赤峰出入境检验检疫局 | Method for detecting residues of carbendazol and thiabendazole in fruit and vegetable juice by high performance liquid chromatography |
| CN105699513B (en) * | 2016-01-21 | 2018-01-30 | 中华人民共和国赤峰出入境检验检疫局 | The method of carbendazim and probenazole residual quantity in high performance liquid chromatography detection Juice |
| CN108572227A (en) * | 2018-06-22 | 2018-09-25 | 苏州仁益生物科技有限公司 | A kind of vegetables detection remaining method of carbendazim of agricultural |
| CN110186914A (en) * | 2018-08-08 | 2019-08-30 | 珠海市慧康生物科技有限公司 | A kind of fruit press and Fast Determination of Pesticide Residue all-in-one machine and detection method |
| CN112461808A (en) * | 2019-09-06 | 2021-03-09 | 苏州市农产品质量安全监测中心 | Detection method and kit for detecting carbendazim in agricultural products |
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Application publication date: 20150422 |