CN102692468A - Reagent kit for detecting pretreatment of common bactericide in perilla leaf, and method thereof - Google Patents

Reagent kit for detecting pretreatment of common bactericide in perilla leaf, and method thereof Download PDF

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Publication number
CN102692468A
CN102692468A CN2012101601340A CN201210160134A CN102692468A CN 102692468 A CN102692468 A CN 102692468A CN 2012101601340 A CN2012101601340 A CN 2012101601340A CN 201210160134 A CN201210160134 A CN 201210160134A CN 102692468 A CN102692468 A CN 102692468A
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reagent
magnesium sulfate
anhydrous magnesium
potpourri
reagent pipe
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陈其勇
肖亚兵
陈旭艳
韩红芳
王云凤
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Tianjin Entry Exit Inspection and Quarantine Bureau of Animals Plants and Food Inspection Center
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Tianjin Entry Exit Inspection and Quarantine Bureau of Animals Plants and Food Inspection Center
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Abstract

The invention relates to a reagent kit for detecting pretreatment of common bactericide in perilla leaf, and a method of for detecting the retreatment of the common bactericide in the perilla leaf, belonging to the technical field of food detection. The kit comprises a case, a reagent tube A, a reagent tube B, a reagent tube C, a reagent tube D, and a filter. The pretreatment method comprises the steps of (1) placing perilla lea into the reagent tube A filled with acetonitrile solution of acetic acid, adding water, adding mixture of anhydrous magnesium sulfate and sodium chloride, or adding mixture of anhydrous magnesium sulfate and sodium acetate, and ultrasonic-extracting; (2) adding mixture of sodium citrate and sodium hydrogen citrate sesquihydrate, oscillating and centrifuging; (3) transferring supernatant to the reagent tube D filled with mixture of N-propyl ethylenediamine (PSA), C18 and anhydrous magnesium sulfate, swirling, and centrifuging; and (4) filtering the supernatant, and performing liquid chromatography-tandem mass spectrometry (LC-MS/MS) detection. The kit has the advantages of simple process, no pollution, room temperature storage, low reagent consumption, high speed, low cost, high accuracy and reliability.

Description

Common fungicide pretreatment reagent kit and method thereof in a kind of detection perilla leaf
Technical field
The invention belongs to the food inspection technical field, particularly relate to common fungicide pretreatment reagent kit and method thereof in a kind of detection perilla leaf.
Background technology
At present, perilla leaf is a kind of product of integration of drinking and medicinal herbs, in people's life, has special status.As a kind of common Chinese herbal medicine, it can play as inducing sweat diffusing cold, and the curative effect of relieving QI stagnancy in the stomach is mainly used in anemofrigid cold, the evil of vomitting of coughing, and the vomiting of pregnancy, the fish crab poisons; As one of rare special vegetable kind, dip in condiment and eat because perilla leaf is mainly used in the volume raw fish, therefore the health to its product requires very strictness with residues of pesticides.Common persticide residue detects and seems very urgent in the perilla leaf.
Purple perilla production germifuge commonly used mainly contains agricultural chemicals such as Difenoconazole, Fluoxastrobin, thiophanate methyl, procymidone.In order to improve the efficient that the common fungicide residual quantity detects in the perilla leaf; Practice thrift and detect cost; Promote the sound development of perilla leaf foreign trade, protection consumer's health, common fungicide pretreatment reagent kit and detection method become important economy and the social concern of being badly in need of solution in the perilla leaf.
Summary of the invention
The present invention provides common fungicide pretreatment reagent kit and method thereof in a kind of detection perilla leaf for solving the technical matters that exists in the known technology.
One of the object of the invention provides a kind of low price that has, and obtain easily, and consumption is little, and sample preparation need not to carry out sample purification with solid phase extraction column, and it is low to detect cost; Kit is easy to operate comfortable, is applicable to the processing of a large amount of dried perilla leaf samples, and the efficient of sample pre-treatments is high, be easy to carry and the detection perilla leaf of characteristics such as storage in the common fungicide pretreatment reagent kit.
The present invention detects the technical scheme that the common fungicide pretreatment reagent kit is taked in the perilla leaf:
Common fungicide pretreatment reagent kit in a kind of detection perilla leaf is characterized in: kit is made up of box body, reagent pipe A, reagent pipe B, reagent pipe C, reagent pipe D and filtrator; Reagent among the reagent pipe A is the acetate acetonitrile solution; Reagent among the reagent pipe B is the potpourri of anhydrous magnesium sulfate and sodium chloride or the potpourri of anhydrous magnesium sulfate and sodium acetate; Reagent among the reagent pipe C is the potpourri of sodium citrate and disodium citrate sesquialter hydrate; Reagent among the reagent pipe D is the potpourri of N--propyl group ethylenediamine (PSA), C18 and anhydrous magnesium sulfate.
The present invention detects in the perilla leaf common fungicide pretreatment reagent kit can also take following technical measures:
Common fungicide pretreatment reagent kit and method thereof in the described detection perilla leaf are characterized in: the weight percent concentration of acetate acetonitrile is 0.5-1%.
Common fungicide pretreatment reagent kit and method thereof in the described detection perilla leaf are characterized in: filtrator is the needle tube type filtrator.
Two of the object of the invention provide a kind of have carry out target compound within a short period of time and measure, practiced thrift detection time greatly and detected cost; Have fast, accurately, detect delicately, easy to operate comfortable, be applicable to the processing of a large amount of dried perilla leaf samples, the method for common fungicide pre-treatment in the detection perilla leaf of characteristics such as the efficient height of sample pre-treatments.
The present invention detects the technical scheme that the method for common fungicide pre-treatment in the perilla leaf takes:
A kind of method that detects common fungicide pre-treatment in the perilla leaf is characterized in: the method for pre-treatment may further comprise the steps:
(1) perilla leaf is put into the reagent pipe A that the acetate acetonitrile solution is housed, add anhydrous magnesium sulfate and the potpourri of sodium chloride or the potpourri of anhydrous magnesium sulfate and sodium acetate among entry and the reagent pipe B, ultrasonic Extraction;
(2) sodium citrate among the adding reagent pipe C and the potpourri of disodium citrate sesquialter hydrate, concussion, centrifugal;
(3) supernatant in the step (2) is transferred among the reagent pipe D of the potpourri that N-propyl group ethylenediamine (PSA), C18 and anhydrous magnesium sulfate are housed, vortex, centrifugal;
(4), carry out the liquid chromatography-tandem mass spectrometry method and detect with behind the supernatant liquid filtering in the step (3).
The present invention detects the method for common fungicide pre-treatment in the perilla leaf can also take following technical measures:
The method of common fungicide pre-treatment in the described detection perilla leaf is characterized in: in the step (1), the ultrasonic Extraction time is 5-20min; In the step (2), concussion time 0.5-2min, centrifugal condition 6000-10000r/min time 3-8min; In the step (3), vortex time 0.5-2min, centrifugal 3-8min under the 6000-10000r/min condition; Filter in the step (4) and adopt the needle tube type filtrator.
The method of common fungicide pre-treatment in the described detection perilla leaf is characterized in: perilla leaf sample and each reagent proportioning are:
In the step (1), take by weighing the perilla leaf sample 3-8g that pulverizes behind the mixing in 50ml reagent pipe A, reagent pipe A is equipped with 0.5-1% acetate acetonitrile solution 10-20ml; Add anhydrous magnesium sulfate and the potpourri of sodium chloride or the potpourri of anhydrous magnesium sulfate and sodium acetate among 6-10mL water and the reagent pipe B; The weight proportion of the potpourri of anhydrous magnesium sulfate and sodium chloride is 5g:1-2g, and the weight proportion of the potpourri of anhydrous magnesium sulfate and sodium acetate is 5g:1-2g.
In the step (2), the mixture weight proportioning of sodium citrate and disodium citrate sesquialter hydrate is 1g:0.5-1g among the reagent pipe C;
In the step (3), the mixture weight proportioning of N-propyl group ethylenediamine (PSA), C18 and anhydrous magnesium sulfate is 200-300mg:200-300mg:1000mg among the reagent pipe D.
Advantage and good effect that the present invention has are:
Common fungicide pretreatment reagent kit and method thereof are owing to adopted brand-new technology scheme of the present invention in the detection perilla leaf; Compared with prior art, the present invention detects the sample pre-treatments kit of common fungicide in the dried perilla leaf (Difenoconazole, Fluoxastrobin, thiophanate methyl, procymidone), sample pre-treatments agents useful for same low price; Obtain easily; And consumption is little, and sample preparation need not to carry out sample purification with solid phase extraction column, thereby has practiced thrift the detection cost greatly; This kit is easy to operate comfortable, is applicable to the processing of a large amount of dried perilla leaf samples, thereby has improved the efficient of sample pre-treatments greatly; This kit is integrated in required reagent and is easy to carry in the pre-treatment box and stores.
The detection method of germifuge (Difenoconazole, Fluoxastrobin, thiophanate methyl, procymidone) in the sample after this pretreatment reagent kit is handled; The moving phase configuration is simple; Can carry out target compound within a short period of time and measure, thereby practice thrift detection time greatly and detected cost.From using the effect of this pretreatment reagent kit and detection method, impurity can be handled totally in the sample.This method be a kind of can be fast, detect the high performance liquid chromatography-tandem mass method (UPLC-MS/MS) of utilizing this pretreatment reagent kit to handle sample accurately, delicately.Advantage of the present invention and characteristics:
(1) simple, pollution-free, the room temperature preservation of the how residual pretreatment reagent kit production run of common fungicide in the perilla leaf disclosed by the invention, the agents useful for same amount is few.
(2) pre-treatment process need not to carry out sample purification with solid phase extraction column, has that speed is fast, cost is low, accuracy and high characteristics of reliability.
(3) added sodium citrate and sesquialter hydration sodium citrate in the kit as the buffer protection agent, can promote separation the responsive agricultural chemicals of soda acid in the perilla leaf.
(4) detection method is for set up first, and it is few to consume reagent, and analysis time is short, can target compound effectively be separated.
Description of drawings
Fig. 1 is the structural representation that the present invention detects common fungicide pretreatment reagent kit in the perilla leaf;
Fig. 2 is the sample after this kit is handled, the mass spectrogram of four kinds of germifuge in the perilla leaf sample that after this detection method detects, draws.
Among the figure, 1, reagent pipe A, 2, reagent pipe B, 3, reagent pipe C, 4, reagent pipe D, 5, disposable needle tubing filtrator.
Embodiment
For further understanding summary of the invention of the present invention, characteristics and effect, the following examples of giving an example now, and conjunction with figs. specifies as follows:
Consult accompanying drawing 1 to Fig. 2.
Embodiment 1
Common fungicide pretreatment reagent kit in a kind of detection perilla leaf is made up of box body, reagent pipe A, reagent pipe B, reagent pipe C, reagent pipe D and needle tube type filtrator E; Wherein, reagent A is contained in the 50mL tool plug screw top polypropylene centrifuge tube, and reagent pipe C is contained in the 5mL tool plug screw top polypropylene centrifuge tube, and reagent D is contained in the 15mL tool plug screw top polypropylene centrifuge tube.
The preparation of kit:
The preparation of reagent A
Preparation 0.5-1% glacial acetic acid mixing acetonitrile solution 10mL is transferred in the 50mL tool plug screw top polypropylene centrifuge tube.
The preparation of reagent B
Take by weighing 2g sodium chloride or sodium acetate and fully mix, be transferred in the sealed reagent bag with the 5g anhydrous magnesium sulfate.
The preparation of reagent C
Taking by weighing 1g sodium citrate and 0.5g disodium citrate sesquialter hydrate is transferred in the 5mL tool plug screw top polypropylene centrifuge tube.
The preparation of reagent D
Take by weighing to 300mg N-propyl group ethylenediamine (PSA), 200mg C18 and 1g anhydrous magnesium sulfate and be transferred in the 15mL tool plug screw top polypropylene centrifuge tube.
Embodiment 2
Application implementation, a kind of method that detects common fungicide pre-treatment in the perilla leaf:
1, get common fungicide pretreatment reagent kit in the perilla leaf, the inside is furnished with reagent pipe A, reagent pipe B, reagent pipe C, reagent pipe D and needle tube type filtrator E.
2, take by weighing the perilla leaf sample 5.0g that pulverizes behind the mixing in reagent pipe A, add 8mL water and reagent pipe B, ultrasonic Extraction 10min; Described reagent pipe A is a 0.5-1% acetate acetonitrile solution; Any one of the potpourri of potpourri, anhydrous magnesium sulfate and sodium acetate that described reagent pipe B is anhydrous magnesium sulfate and sodium chloride;
3, add reagent pipe C, concuss 1min, the centrifugal 5min of 8000r/min; The potpourri of described reagent pipe C sodium citrate and disodium citrate sesquialter hydrate;
4, supernatant is transferred among the reagent pipe D vortex 1min, the centrifugal 5min of 8000r/min; Described reagent pipe D is the potpourri of N-propyl group ethylenediamine (PSA), C18 and anhydrous magnesium sulfate;
5, supernatant supplies UPLCMS/MS to detect after needle tube type filtrator E filters.
Embodiment 3
Application implementation, a kind of method that detects common fungicide pre-treatment in the perilla leaf:
1, will use pretreatment reagent kit processing back perilla leaf sample measures by following liquid chromatography-tandem mass spectrometry condition.
2, preferred chromatographic condition: chromatographic column: ACQUITY UPLC BEH C18 post, 2.1 * 10mm, 1.7 μ m; Column temperature: 25 ℃; Sample size: 2 μ L; Flow velocity: 0.25mL/min.Condition of gradient elution: A is methyl alcohol mutually, and B is the 10mmol/L ammonium acetate mutually, 0~3min, 20%A; 3~4min, 90%A; 4~5min, 90%A; 5~6min, 20%A.
3, preferred mass spectrum condition: ion gun: electric spray ion source; Scan mode: positive ion scanning; Drainage pattern: multiple-reaction monitoring pattern MRM; Capillary voltage: 3.12kV; Desolventizing temperature degree: 400 ℃; Desolventizing gas velocity: 800L/Hr; Taper hole blowback air flow velocity: 50L/Hr; Agricultural chemicals to be measured is qualitative, quota ion is seen table 1 to taper hole voltage and collision voltage.
Table 1 agricultural chemicals to be measured is qualitative, quota ion is to taper hole voltage and collide voltage
Figure BDA00001666589200051
Annotate: what * marked is quota ion.
Common fungicide pretreatment reagent kit and method thereof have advantage of the present invention and good effect in the present embodiment detection perilla leaf.

Claims (6)

1. one kind is detected common fungicide pretreatment reagent kit in the perilla leaf, and it is characterized in that: kit is made up of box body, reagent pipe A, reagent pipe B, reagent pipe C, reagent pipe D and filtrator; Reagent among the reagent pipe A is the acetate acetonitrile solution; Reagent among the reagent pipe B is the potpourri of anhydrous magnesium sulfate and sodium chloride or the potpourri of anhydrous magnesium sulfate and sodium acetate; Reagent among the reagent pipe C is the potpourri of sodium citrate and disodium citrate sesquialter hydrate; Reagent among the reagent pipe D is the potpourri of N-propyl group ethylenediamine (PSA), C18 and anhydrous magnesium sulfate.
2. common fungicide pretreatment reagent kit in the detection perilla leaf according to claim 1 is characterized in that: the weight percent concentration of acetate acetonitrile is 0.5-1%.
3. common fungicide pretreatment reagent kit in the detection perilla leaf according to claim 1 is characterized in that: filtrator is the needle tube type filtrator.
4. method that detects common fungicide pre-treatment in the perilla leaf, it is characterized in that: the method for pre-treatment may further comprise the steps:
(1) perilla leaf is put into the reagent pipe A that the acetate acetonitrile solution is housed, add anhydrous magnesium sulfate and the potpourri of sodium chloride or the potpourri of anhydrous magnesium sulfate and sodium acetate among entry and the reagent pipe B, ultrasonic Extraction;
(2) sodium citrate among the adding reagent pipe C and the potpourri of disodium citrate sesquialter hydrate, concussion, centrifugal;
(3) supernatant in the step (2) is transferred among the reagent pipe D of the potpourri that N-propyl group ethylenediamine (PSA), C18 and anhydrous magnesium sulfate are housed, vortex, centrifugal;
(4), carry out the liquid chromatography-tandem mass spectrometry method and detect with behind the supernatant liquid filtering in the step (3).
5. the method for common fungicide pre-treatment in the detection perilla leaf according to claim 4 is characterized in that: in the step (1), the ultrasonic Extraction time is 5-20min; In the step (2), concussion time 0.5-2min, centrifugal condition 6000-10000r/min time 3-8min; In the step (3), vortex time 0.5-2min, centrifugal 3-8min under the 6000-10000r/min condition; Filter in the step (4) and adopt the needle tube type filtrator.
6. according to the method for common fungicide pre-treatment in claim 4 or the 5 described detection perilla leafs, it is characterized in that: perilla leaf sample and each reagent proportioning are:
In the step (1), take by weighing the perilla leaf sample 3-8g that pulverizes behind the mixing in 50ml reagent pipe A, reagent pipe A is equipped with 0.5-1% acetate acetonitrile solution 10-20ml; Add anhydrous magnesium sulfate and the potpourri of sodium chloride or the potpourri of anhydrous magnesium sulfate and sodium acetate among 6-10mL water and the reagent pipe B; The weight proportion of the potpourri of anhydrous magnesium sulfate and sodium chloride is 5g:1-2g, and the weight proportion of the potpourri of anhydrous magnesium sulfate and sodium acetate is 5g:1-2g.
In the step (2), the mixture weight proportioning of sodium citrate and disodium citrate sesquialter hydrate is 1g:0.5-1g among the reagent pipe C;
In the step (3), the mixture weight proportioning of N-propyl group ethylenediamine (PSA), C18 and anhydrous magnesium sulfate is 200-300mg:200-300mg:1000mg among the reagent pipe D.
CN2012101601340A 2012-05-22 2012-05-22 Reagent kit for detecting pretreatment of common bactericide in perilla leaf, and method thereof Pending CN102692468A (en)

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CN103512993A (en) * 2013-10-12 2014-01-15 崔淑华 Hot pepper and determining method for 96 pesticide residues in product of hot pepper
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CN107917996A (en) * 2017-10-19 2018-04-17 安徽省东博米业有限公司 A kind of finished product rice multifunctional detecting device and its application method

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103412077A (en) * 2013-07-14 2013-11-27 崔淑华 Method for measuring indazole flusulfamide residue amount
CN103512993A (en) * 2013-10-12 2014-01-15 崔淑华 Hot pepper and determining method for 96 pesticide residues in product of hot pepper
CN104407090A (en) * 2014-12-30 2015-03-11 郭庆龙 Method for determining residue of spirotetramat in fruits and vegetables by GC-NCI-MS (gas chromatography-negative chemical ionization-mass spectrometry)
CN104458968A (en) * 2014-12-30 2015-03-25 郭庆龙 GC-EI-MS (gas chromatography-electron impact ionization-mass spectrometry) measuring method of residual quantity of spirotetramat in fruit and vegetable
CN104502505A (en) * 2014-12-30 2015-04-08 郭庆龙 GC-EI-MS (Gas Chromatography-Electron Ionization-Mass Spectrum) detecting method for residual quantity of spirotetramat
CN104502506A (en) * 2014-12-30 2015-04-08 郭庆龙 GC-NCI-MS (Gas Chromatography-Negative Chemical Ionization-Mass Spectrum) detecting method for residual quantity of spirotetramat
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CN104407090B (en) * 2014-12-30 2015-12-09 郭庆龙 A kind of GC-NCI-MS measures the method that in fruits and vegetables, spiral shell worm ethyl ester is residual
CN104502506B (en) * 2014-12-30 2015-12-09 郭庆龙 A kind of GC-NCI-MS assay method of spiral shell worm ethyl ester residual quantity
CN104502505B (en) * 2014-12-30 2015-12-30 郭庆龙 A kind of GC-EI-MS assay method of spiral shell worm ethyl ester residual quantity
CN107917996A (en) * 2017-10-19 2018-04-17 安徽省东博米业有限公司 A kind of finished product rice multifunctional detecting device and its application method

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Application publication date: 20120926