CN104569163A - Technology for simultaneous determination of kresoxim-methyl and trifloxystrobin of orange by QuEChERS-HPLC - Google Patents
Technology for simultaneous determination of kresoxim-methyl and trifloxystrobin of orange by QuEChERS-HPLC Download PDFInfo
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- CN104569163A CN104569163A CN201310472907.3A CN201310472907A CN104569163A CN 104569163 A CN104569163 A CN 104569163A CN 201310472907 A CN201310472907 A CN 201310472907A CN 104569163 A CN104569163 A CN 104569163A
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- kresoxim
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- oxime bacterium
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Abstract
Kresoxim-methyl and trifloxystrobin belong to Strobilurin bactericides, has the characteristics of low toxicity, high efficiency and wide spectrum and can be widely used in the field of crops and fungous disease prevention and treatment by a unique action mechanism. The problem that orange-type fruits easily decay is regarded as a global issue attracting worldwide attention. Penicilliosis and penicillium digitatum are common in orange storage. Kresoxim-methyl and trifloxystrobin have good activity to human diseases caused by pathogenic fungi such as blue mold and green mold. Penicilliosis and penicillium digitatum have been produced in China and been used in prevention and treatment on orange diseases. A QuEchERS method is a pre-treatment method for pesticide multiresidual analysis. A high performance liquid chromatography is a general technology for pesticide residue detection and is suitable for a base detection mechanism. Through the QuEChERS-HPLC method, residues of two strobilurin bactericides such as kresoxim-methyl and trifloxystrobin in oranges are detected. The technology has the characteristics of simpleness, fastness, safety, low price and wide adaptability.
Description
Technical field
QuEchERS method is a kind of easy, quick, safe, the cheap pre-treating method in Multi-residue analysis.The analysis and detection technology being applied to Strobilurin series bactericidal agent residual mainly contains gas chromatography (GC), high performance liquid chromatography (HPLC), combined gas chromatography mass spectrometry (GC/MS, HPLC-MS), enzyme-linked immuno assay (ELISA) etc.
The present invention relates to and detect 2 kinds of strobilurin germifuge in oranges and tangerines by QuEChERS-HPLC method simultaneously----kresoxim-methyl and oxime bacterium ester residual, this technology has feature that is easy, quick, safe, cheap and wide adaptability.
Background technology
Sample pre-treatments object is by component extraction to be measured, purification and enrichment.It is the principal element that impact detects analytical error, can say that the analytical error caused due to pre-treatment is considerably beyond the analytical error brought by instrument itself.Usually our sample substrate of analyzing and processing is more complicated, and the method for good pre-treatment can effectively reduce even avoids matrix effect to analyzing the interference brought.Along with the development of science and technology, pretreatment technology is also to simple, quick, cheap, environmental friendliness aspect development.QuEchERS method is a kind of easy, quick, safe, the cheap analytical approach in Multi-residue analysis.The key step of the method carries out lixiviate with the acetonitrile containing 1% acetic acid to sample, add anhydrous magnesium sulfate and sodium acetate again to vibrate and impel its layering, carry out dispersive solid-phase extraction subsequently, be transferred in the centrifuge tube containing PSA adsorbent, magnesium sulfate by leaching liquor, use Teflon coating centrifuge tube to carry out centrifugal, extracting centrifugal liquid is used for measuring to auto injection bottle.QuEchERS method and can use the difference of medium suitably to adjust according to the scope of alternative analytical instrument kind, detectability, target agricultural chemicals.
Kresoxim-methyl and oxime bacterium ester belong to Strobilurin series bactericidal agent, have the feature of low toxicity, efficient, wide spectrum, are widely used in crops and control fungal disease field with the mechanism of action of its uniqueness.Citrus fruit is adopted rear perishable, causes in world wide greatly pay close attention to as a global problem.Oxime bacterium ester and kresoxim-methyl have good activity to most of diseases that pathomycete causes, and as the representative of methoxy acrylic bactericide, are used for the disease control of oranges and tangerines in China.
Because the pre-treating method applying to retention analysis is more, suitable pre-treating method is therefore selected to analyze thing to enrich target very important.The residual conventional high-speed homogenization method of the object of Strobilurin series bactericidal agent in fruit and vegetable is slightly carried, in cereal, then select mechanical shaking extraction, and microwave and ultrasound also can be used for this series bactericidal agent and slightly extracts in addition.QuEchERS method is a kind of easy, quick, safe, the cheap analytical approach in Multi-residue analysis.
Summary of the invention
The invention discloses 2 kinds of strobilurin germifuge---the technical method of kresoxim-methyl and oxime bacterium ester utilized in QuEChERS method extraction oranges and tangerines.
The invention discloses and utilize high performance liquid chromatography to detect 2 kinds of strobilurin germifuge---the technical method of kresoxim-methyl and oxime bacterium ester in oranges and tangerines simultaneously.
Accompanying drawing explanation
The typical curve of Fig. 1 kresoxim-methyl (left side) and oxime bacterium ester (right side)
Fig. 2 kresoxim-methyl and oxime bacterium ester HPLC detect collection of illustrative plates: mix the orange peel sample after tangerine meat sample (d) orange peel blank sample (e) drug treating after mark product collection of illustrative plates (b) tangerine meat blank sample (c) drug treating under (a) MRL level
1-kresoxim-methyl, 2-oxime bacterium ester
Kresoxim-methyl and oxime bacterium ester TIANZHU XINGNAO Capsul and RSD% in Fig. 3 oranges and tangerines
embodiment
The method for detecting residue of 1 kresoxim-methyl and oxime bacterium ester
The extraction of 1.1 kresoxim-methyls and oxime bacterium ester
Adopt the QuEChERS method determined in conjunction with AOAC and CEN standard method.The acetonitrile containing 1% acetic acid with 10ml joins 10g sample (meat, skin), homogenate adds 4g anhydrous magnesium sulfate and 1g anhydrous sodium acetate after extracting, vibrate centrifugal, every milliliter of supernatant adds in 150mg anhydrous magnesium sulfate and 20mg PSA and 5mg C18, and vortex oscillation is centrifugal, supernatant nitrogen dries up, mobile phase is fixed molten, crosses 0.22um miillpore filter, treats machine examination.
The detection of 1.2 kresoxim-methyls and oxime bacterium ester
The determination of liquid chromatography correlation parameter.Maximum absorption wavelength: kresoxim-methyl and oxime bacterium ester mark solution are done UV scanning, determines that the optimal wavelength that both detect simultaneously is 210nm.Detected temperatures: 40 DEG C.Flow velocity: 1ml/min.Mobile phase: first alcohol and water (80:20).By the standard solution that standard stock solution dilution is 0.05,0.25,1,2,5,10,20,50ug/ml, after crossing film process, machine testing in often kind of concentration 10uL sampling take concentration as horizontal ordinate, peak area is ordinate drawing standard curve (Fig. 1).Kresoxim-methyl typical curve equation is y=10596x-479.94, R
2=0.9996; Oxime bacterium ester typical curve equation is y=11206x-328.13, R
2=0.9999.The retention time of kresoxim-methyl and oxime bacterium ester is respectively at about 9.3min and about 12.3min (Fig. 2).
The Accuracy Verification of 1.3 methods
10g blank sample (orange peel and tangerine meat) makes interpolation concentration reach 0.05,0.5,1mg/kg at middle interpolation kresoxim-methyl and oxime bacterium ester standard solution.Each concentration parallel laboratory test 5 times.The method in 1.1 and 1.2 is adopted to carry out pre-treatment and chromatogram detection, the recovery and relative standard deviation, result Fig. 3.In this method, the LOD value of kresoxim-methyl and oxime bacterium ester is 0.005 and 0.008mg/kg; LOQ value is 0.010 and 0.012mg/kg.
Claims (3)
1. apply the technology of kresoxim-methyl and oxime bacterium ester in QuEChERS-HPLC Simultaneously test oranges and tangerines, comprise following content:
(1) utilize QuEChERS method to extract the technology of kresoxim-methyl and oxime bacterium ester in oranges and tangerines simultaneously
(2) HPLC of oxime bacterium ester, kresoxim-methyl detection technique simultaneously in oranges and tangerines.
2. the QuEChERS method that utilizes according to claim 1 extracts kresoxim-methyl and oxime bacterium ester in oranges and tangerines, according to the characteristic of kresoxim-methyl and oxime bacterium ester, select PSA and ODS (4/1, m/m) carry out dispersive solid-phase extraction as adsorbent, the oranges and tangerines sample containing kresoxim-methyl and oxime bacterium fat is purified.
3. the HPLC Simultaneous Detection of oxime bacterium ester, kresoxim-methyl in oranges and tangerines according to claim 1, is characterized in that kresoxim-methyl has relative absorption maximum with oxime bacterium ester at 210nm, is defined as optimum and detects absorbing wavelength simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310472907.3A CN104569163A (en) | 2013-10-11 | 2013-10-11 | Technology for simultaneous determination of kresoxim-methyl and trifloxystrobin of orange by QuEChERS-HPLC |
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| CN201310472907.3A CN104569163A (en) | 2013-10-11 | 2013-10-11 | Technology for simultaneous determination of kresoxim-methyl and trifloxystrobin of orange by QuEChERS-HPLC |
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| CN104569163A true CN104569163A (en) | 2015-04-29 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770841A (en) * | 2017-03-23 | 2017-05-31 | 西北师范大学 | The method that fruit Pesticides Testing sample is processed using QuEChERS abstraction techniques |
| CN106770725A (en) * | 2016-11-29 | 2017-05-31 | 通标标准技术服务(上海)有限公司 | A kind of method of dinocap residual quantity in quick measure vegetable and fruit |
| CN109001312A (en) * | 2018-07-04 | 2018-12-14 | 上海德易检测技术有限公司 | A kind of detection method of pesticide residues in fruits |
| CN113109559A (en) * | 2021-03-23 | 2021-07-13 | 宁波市农业科学研究院 | Immunochromatography gold-labeled test strip suitable for trifloxystrobin pesticide and rapid test method thereof |
-
2013
- 2013-10-11 CN CN201310472907.3A patent/CN104569163A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| FARAG MALHAT等: "Residues and dissipation of kresoxim methyl in apple under field condition", 《FOOD CHEMISTRY》 * |
| JIE ZHU等: "Simultaneous detection and degradation patterns of kresoxim-methyl and trifloxystrobin residues in citrus fruits by HPLC combined with QuEChERS", 《JOURNAL OF ENVIRONMENTAL SCIENCE AND HEALTH, PART B》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770725A (en) * | 2016-11-29 | 2017-05-31 | 通标标准技术服务(上海)有限公司 | A kind of method of dinocap residual quantity in quick measure vegetable and fruit |
| CN106770725B (en) * | 2016-11-29 | 2019-04-16 | 通标标准技术服务(上海)有限公司 | A kind of method of dinocap residual quantity in quick measurement vegetable and fruit |
| CN106770841A (en) * | 2017-03-23 | 2017-05-31 | 西北师范大学 | The method that fruit Pesticides Testing sample is processed using QuEChERS abstraction techniques |
| CN109001312A (en) * | 2018-07-04 | 2018-12-14 | 上海德易检测技术有限公司 | A kind of detection method of pesticide residues in fruits |
| CN113109559A (en) * | 2021-03-23 | 2021-07-13 | 宁波市农业科学研究院 | Immunochromatography gold-labeled test strip suitable for trifloxystrobin pesticide and rapid test method thereof |
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Application publication date: 20150429 |