CN1483500A - Column for purifying pesticide residue and purification method thereof - Google Patents
Column for purifying pesticide residue and purification method thereof Download PDFInfo
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- CN1483500A CN1483500A CNA031537251A CN03153725A CN1483500A CN 1483500 A CN1483500 A CN 1483500A CN A031537251 A CNA031537251 A CN A031537251A CN 03153725 A CN03153725 A CN 03153725A CN 1483500 A CN1483500 A CN 1483500A
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- decontaminating column
- purification method
- pesticides
- residues
- filler
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Abstract
The present invention relates to a pesticide residue cleaning column with mixed filler and its cleaning method. Said clenaing column includes external shell, upper screen plate, low screen plate and filler, the described upper screen plate is positioned in upper portion of the internal space of the external shell of the cleaning column, the lower screen plate is positioned in the bottom portion of external shell of the cleaning column, and the filler is positioned between upper and lower screen plates, and the composition of said filler includes (wt%) 1%-30% of active carbon, 40%-80% of diatomaceous earth and 15%-45% of filter aid, and the grain size range of said mixed filler is 5 micrometers-100 micrometers.
Description
Technical field
The present invention relates to a kind of chemical analysis process tower, relate in particular to a kind of residues of pesticides decontaminating column and purification method thereof that mixed fillers is housed.
Background technology
It is in order accurately to detect residual medicine and banned substance in food, the agricultural product in the down-stream that the remains of pesticide that extracts from food is purified, it is simple to carry out the inner adsorption stuffing composition of various decontaminating columns that this purification adopts at present, as C18, C8, NH2, CN, Si, Al or organic polymer etc. are only arranged, this adsorption stuffing is suitable for a kind of or alanysis thing absorption, being not suitable for multicomponent handles, therefore the decontaminating column and the purification method processing time thereof of prior art are long, be of limited application, cost is higher.
Summary of the invention
Purpose of the present invention is exactly to overcome these defectives that exist in the prior art, and providing a kind of can independently use, and can adsorb and purify the residues of pesticides decontaminating column and the purification method of multiclass medicine simultaneously.
For achieving the above object, the invention provides a kind of like this residues of pesticides decontaminating column, it comprises shell, upper sieve plate, following sieve plate and mixed fillers, described upper sieve plate is positioned at decontaminating column enclosure space than top, following sieve plate is positioned at the decontaminating column outer casing bottom, mixed fillers is between described up and down sieve plate, described mixed fillers constitutes (percentage by weight) by following component: active carbon 1%-30%, diatomite 40%-80%, filter aid 15%-45%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
Further described plate thickness is 2mm, and sieve plate is the network with certain pore size, and physicochemical properties are stable, can prevent that filler from coming out, and can stop big particle diameter material to enter again.
Further, described mixed fillers constitutes (percentage by weight) by following component: active carbon 5%, and diatomite 60%, filter aid 35%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
Further, described mixed fillers constitutes (percentage by weight) by following component: active carbon 10%, and diatomite 75%, filter aid 15%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
Further, described mixed fillers constitutes (percentage by weight) by following component: active carbon 20%, and diatomite 60%, filter aid 20%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
Further, described mixed fillers constitutes (percentage by weight) by following component: active carbon 25%, and diatomite 50%, filter aid 25%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
The present invention also provides a kind of residues of pesticides purification method, and this method comprises the following steps:
(1) prepares decontaminating column, according to being cleaned sample configuration decontaminating column filler;
(2) preparation sample solution;
(3) activation of decontaminating column adds decontaminating column in from decontaminating column top activator and flows through decontaminating column, discards outflow liquid;
(4) go up sample, sample solution is added in the decontaminating column;
(5) wash-out of decontaminating column adds eluant, eluent from the decontaminating column top, collect and flow out liquid, and is to be checked;
Whole process liquids flow velocity is no more than 4ml/min.
Further, the step in above-mentioned purification method (4) can also be carried out the washing step of decontaminating column afterwards, after dose outflow promptly to be activated, adds washing agent from the decontaminating column top, and washing agent flows through from decontaminating column, removes impurity wherein effectively, discards outflow liquid.
Further, after washing agent flows through decontaminating column, adopt malleation to blow, utilize malleation that residual impurity is blown out, perhaps adopt the negative pressure suction, the residual impurity sucking-off in the decontaminating column bottom on decontaminating column top.
Further, described purification method is used for the residual organophosphorus insecticide that extracts in the decontaminate food, and its used decontaminating column filler component is (percentage by weight): active carbon 10%, diatomite 75%, filter aid 15%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
Further, described purification method is used for the residual organophosphorus insecticide that extracts in the decontaminate food, and activator adopts acetone and n-hexane mixed liquor, and wherein the ratio between acetone and the n-hexane (volume) is 1: 99-40: 60.
Further, described purification method is used for the residual organophosphorus insecticide that extracts in the decontaminate food, and its used washing agent adopts acetone and n-hexane mixed liquor, and wherein the ratio between acetone and the n-hexane (volume) is 10: 90-50: 50.
Further, described purification method is used for the residual organophosphorus insecticide that extracts in the decontaminate food, and its used eluant, eluent adopts n-hexane and carrene mixed liquor, and wherein the ratio between n-hexane and the carrene (volume) is 50: 50-95: 5.
Further, described purification method is used for the residual organic chlorine agriculture chemicals that extracts in the decontaminate food, and its used decontaminating column filler component is (percentage by weight): active carbon 20%, diatomite 60%, filter aid 20%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
Further, described purification method is used for the residual organic chlorine agriculture chemicals that extracts in the decontaminate food, and its used activator adopts the mixed liquor of water and acetone, and wherein the ratio between water and the acetone (volume) is 90: 10.
Further, described purification method is used for the residual organic chlorine agriculture chemicals that extracts in the decontaminate food, and its used washing agent adopts the mixed liquor of water and acetone, and wherein the ratio between water and the acetone (volume) is 90: 10.
Further, described purification method is used for the residual organic chlorine agriculture chemicals that extracts in the decontaminate food, and its used eluant, eluent adopts acetone.
Further, described purification method is used for the residual carbamate chemicals for agriculture that extracts in the decontaminate food, and its used decontaminating column filler component is (percentage by weight): active carbon 25%, diatomite 50%, filter aid 25%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
Further, described purification method is used for the residual carbamate chemicals for agriculture that extracts in the decontaminate food, and its used activator adopts the mixed liquor of n-hexane and carrene, and wherein the ratio between n-hexane and the carrene (volume) is 35: 65.
Adopt residues of pesticides decontaminating column of the present invention and purification method, can in time purify whole operation process＜20min apace to the liquid to be checked that from food, extracts; And adopting different filler configurations, different washing agent and eluant, eluents to purify to the Multiple Pesticides extract, good purification satisfies the Instrumental Analysis requirement, therefore, the present invention is applied widely, and is convenient to use, with low cost, it is accurate to purify the back testing result.
Description of drawings
Fig. 1 is a residues of pesticides decontaminating column schematic diagram of the present invention.
The specific embodiment
Fig. 1 is a residues of pesticides decontaminating column schematic diagram of the present invention, as shown in the drawing, decontaminating column monnolithic case syringe-like bucket, mixed fillers 4 between sieve plate constitutes by shell 1, upper sieve plate 2, following sieve plate 3 with about placing for it, mixed fillers constitutes (percentage by weight) by following component: active carbon 30%, diatomite 40%, filter aid 30%, above-mentioned filler mixed packing, particle size range is between 5 μ m-60 μ m.The thickness of upper sieve plate 1 and following sieve plate 2 is 2mm, and the mesh-structured physicochemical properties on it are stable, can rise and filter and iris action, prevents that filler from coming out, and stops big particle diameter material to enter.The mechanism of action of residues of pesticides decontaminating column of the present invention is to utilize the suction-operated principle of mixed fillers (oppositely absorption, hydrogen bond, hydrophobic effect etc.), analyte is optionally adsorbed and keeps, after in purification process, utilizing cleaning solvent to remove impurity effectively, with suitable eluant, eluent analysans is eluted targetedly again.
Further describe purification method of the present invention below in conjunction with several pesticide residues that often purify in the practical application.
Embodiment 1 thing to be checked: the agricultural residual drug type of spinach (vegetables with green leaves): organophosphorus insecticide decontaminating column filler configuration: filler 300mg, wherein active carbon 10% (granularity 100 μ m), diatomite 75% (granularity 60 μ m), filter aid (Celite545) 15% (granularity 10 μ m); Purification method comprises the following steps: the first step, and the preparation sample solution is with the analyte in 20ml n-hexane and acetone (volume ratio 50: 50) the mixed liquor extraction spinach; In second step, the activating and purifying post flows through decontaminating column with 20ml n-hexane and acetone (volume ratio 70: 30) mixed liquor; In the 3rd step, last sample adds to the spinach extract in the decontaminating column, blots under the negative pressure; In the 4th step, wash-out flows through decontaminating column with 10ml n-hexane and carrene (volume ratio 50: 50) mixed liquor, blots under the negative pressure, collects eluent.The analyte rate of recovery: 85～97%, relative standard deviation:＜5%.
Embodiment 2 things to be checked: the agricultural residual drug type of pears (fruit): organic chlorine agriculture chemicals prepares the decontaminating column filler, filler 90mg, wherein active carbon 20% (granularity 100 μ m), diatomite 60% (granularity 60 μ m), filter aid (Celite545) 20% (granularity 10 μ m); Purification method comprises the following steps: the first step, and the preparation sample solution is with the analyte in 10ml water and acetone (volume ratio 40: 60) the mixed liquor extraction pears; In second step, the activating and purifying post flows through decontaminating column with 10ml water and acetone (volume ratio 90: 10) mixed liquor; In the 3rd step, last sample adds to the pears extract in the decontaminating column; In the 4th step, washing is flow through decontaminating column with 10ml water and acetone (volume ratio 90: 10) mixed liquor, blots under the negative pressure; In the 5th step, wash-out flows through decontaminating column with 10ml acetone, blots under the negative pressure, collects eluent.The analyte rate of recovery: 80～99%, relative standard deviation:＜6%.
Embodiment 3 things to be checked: the big residual drug type of garlic farmers: the carbamate chemicals for agriculture decontaminating column filler of purchasing: filler 150mg, wherein active carbon 25% (granularity 100 μ m), diatomite 50% (granularity 60 μ m), filter aid (Celite545) 25% (granularity 10 μ m), purification method comprises the following steps: the first step, the preparation sample solution is with the analyte in 15ml n-hexane and carrene (volume ratio 35: 65) the mixed liquor extraction garlic; In second step, the activating and purifying post flows through decontaminating column with 15ml n-hexane and carrene (volume ratio 35: 65) mixed liquor.The 3rd step, last sample.Garlic extract is added in the decontaminating column, flow through, blot under the negative pressure, collect and flow out liquid.The analyte rate of recovery: 90～98%, relative standard deviation:＜3%.In this embodiment, impurity is attracted on the decontaminating column, and carbamate chemicals for agriculture flows out along with flowing out liquid.
Claims (20)
1, a kind of residues of pesticides decontaminating column, it comprises shell, upper sieve plate, following sieve plate and filler, described upper sieve plate is positioned at decontaminating column enclosure space than top, and following sieve plate is positioned at the decontaminating column outer casing bottom, and filler is between described up and down sieve plate, it is characterized in that, described filler constitutes (percentage by weight) by following component: active carbon 1%-30%, diatomite 40%-80%, filter aid 15%-45%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
2, a kind of residues of pesticides decontaminating column as claimed in claim 1 is characterized in that, described plate thickness is 2mm, and sieve plate is the network with certain pore size, and physicochemical properties are stable, can prevent that filler from coming out, and can stop big particle diameter material to enter again.
3, a kind of residues of pesticides decontaminating column as claimed in claim 1 or 2 is characterized in that described mixed fillers constitutes (percentage by weight) by following component: active carbon 5%, diatomite 60%, filter aid 35%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
4, a kind of residues of pesticides decontaminating column as claimed in claim 1 or 2 is characterized in that described mixed fillers constitutes (percentage by weight) by following component: active carbon 10%, diatomite 75%, filter aid 15%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
5, a kind of residues of pesticides decontaminating column as claimed in claim 1 or 2 is characterized in that described mixed fillers constitutes (percentage by weight) by following component: active carbon 20%, diatomite 60%, filter aid 20%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
6, a kind of residues of pesticides decontaminating column as claimed in claim 1 or 2 is characterized in that described mixed fillers constitutes (percentage by weight) by following component: active carbon 25%, diatomite 50%, filter aid 25%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
7, a kind of residues of pesticides purification method, this method comprises the following steps:
(1) prepares decontaminating column, according to being cleaned sample configuration decontaminating column filler;
(2) preparation sample solution;
(3) activation of decontaminating column adds decontaminating column in from decontaminating column top activator and flows through decontaminating column, discards outflow liquid;
(4) go up sample, sample solution is added in the decontaminating column;
(5) wash-out of decontaminating column adds eluant, eluent from the decontaminating column top, collect and flow out liquid, and is to be checked.
8, a kind of residues of pesticides purification method as claimed in claim 7 is characterized in that, the step in above-mentioned purification method (4) afterwards, carry out the washing step of decontaminating column, treat that promptly sample solution flows out after, add washing agent from the decontaminating column top, washing agent flows through from decontaminating column, discards outflow liquid then.
9, a kind of residues of pesticides purification method as claimed in claim 8 is characterized in that, after described washing agent flows through decontaminating column, utilize malleation to blow on decontaminating column top, utilize malleation that residual impurity is blown out, perhaps adopt the secondary suction of pressing, the residual impurity sucking-off in the decontaminating column bottom.
10, a kind of residues of pesticides purification method, this method comprises the following steps:
(1) prepares decontaminating column, according to being cleaned sample configuration decontaminating column filler;
(2) preparation sample solution;
(3) activation of decontaminating column adds decontaminating column in from decontaminating column top activator and flows through decontaminating column, discards outflow liquid;
(4) go up sample, sample solution is added in the decontaminating column, collect and flow out liquid, to be checked.
11, a kind of residues of pesticides purification method as claimed in claim 10, it is characterized in that, described purification method is used for the residual carbamate chemicals for agriculture that extracts in the decontaminate food, its used decontaminating column filler component is (percentage by weight): active carbon 25%, diatomite 50%, filter aid 25%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
12, a kind of residues of pesticides purification method as claimed in claim 10, it is characterized in that, described purification method is used for purifying the residual carbamate chemicals for agriculture that extracts from food, its used activator adopts the mixed liquor of n-hexane and carrene, and wherein the ratio between n-hexane and the carrene (volume) is 35: 65.
13, a kind of as the described residues of pesticides purification method of arbitrary claim among the claim 7-9, it is characterized in that, described purification method is used for purifying the residual organophosphorus insecticide that extracts from food, its used decontaminating column filler component is (percentage by weight): active carbon 10%, diatomite 75%, filter aid 15%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
14, a kind of as the described residues of pesticides purification method of arbitrary claim among the claim 7-9, it is characterized in that, described purification method is used for purifying the residual organophosphorus insecticide that extracts from food, activator adopts acetone and n-hexane mixed liquor, and wherein the ratio between acetone and the n-hexane (volume) is 1: 99-40: 60.
15, a kind of as the described residues of pesticides purification method of arbitrary claim among the claim 8-9, it is characterized in that, described purification method is used for purifying the residual organophosphorus insecticide that extracts from food, its used washing agent adopts acetone and n-hexane mixed liquor, and wherein the ratio between acetone and the n-hexane (volume) is 10: 90-50: 50.
16, a kind of as the described residues of pesticides purification method of arbitrary claim among the claim 7-9, it is characterized in that, described purification method is used for purifying the residual organophosphorus insecticide that extracts from food, its used eluant, eluent adopts n-hexane and carrene mixed liquor, and wherein the ratio between n-hexane and the carrene (volume) is 50: 50-95: 5.
17, a kind of as the described residues of pesticides purification method of arbitrary claim among the claim 7-9, it is characterized in that, described purification method is used for purifying the residual organic chlorine agriculture chemicals that extracts from food, its used decontaminating column filler component is (percentage by weight): active carbon 20%, diatomite 60%, filter aid 20%, above-mentioned filler mixed packing, particle size range is between 5 μ m-100 μ m.
18, a kind of as the described residues of pesticides purification method of arbitrary claim among the claim 7-9, it is characterized in that, described purification method is used for purifying the residual organic chlorine agriculture chemicals that extracts from food, its used activator adopts the mixed liquor of water and acetone, and wherein the ratio between water and the acetone (volume) is 90: 10.
19, a kind of as the described residues of pesticides purification method of arbitrary claim among the claim 8-9, it is characterized in that, described purification method is used for purifying the residual organic chlorine agriculture chemicals that extracts from food, its used washing agent adopts the mixed liquor of water and acetone, and wherein the ratio between water and the acetone (volume) is 90: 10.
20, a kind ofly it is characterized in that as the described residues of pesticides purification method of arbitrary claim among the claim 7-9 described purification method is used for purifying the residual organic chlorine agriculture chemicals that extracts from food, its used eluant, eluent adopts acetone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03153725 CN1221299C (en) | 2003-08-19 | 2003-08-19 | Column for purifying pesticide residue and purification method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03153725 CN1221299C (en) | 2003-08-19 | 2003-08-19 | Column for purifying pesticide residue and purification method thereof |
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| CN1483500A true CN1483500A (en) | 2004-03-24 |
| CN1221299C CN1221299C (en) | 2005-10-05 |
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| CN 03153725 Expired - Fee Related CN1221299C (en) | 2003-08-19 | 2003-08-19 | Column for purifying pesticide residue and purification method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101549217A (en) * | 2009-04-17 | 2009-10-07 | 天津博纳艾杰尔科技有限公司 | Medicament extracting device and method from body fluid example |
| CN101780396B (en) * | 2010-02-02 | 2012-10-10 | 中国地质大学（武汉） | Absorbing agent of trace organic chloride pesticide in water body and preparation method thereof |
| CN103611334A (en) * | 2013-10-22 | 2014-03-05 | 上海安谱科学仪器有限公司 | Filling method for diatomite column |
| CN104667898A (en) * | 2015-02-06 | 2015-06-03 | 玉林师范学院 | Preparation method of eucalyptus-based porous carbon-silicon dioxide solid-phase extraction column |
-
2003
- 2003-08-19 CN CN 03153725 patent/CN1221299C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101549217A (en) * | 2009-04-17 | 2009-10-07 | 天津博纳艾杰尔科技有限公司 | Medicament extracting device and method from body fluid example |
| CN101549217B (en) * | 2009-04-17 | 2014-05-28 | 天津博纳艾杰尔科技有限公司 | Medicament extracting device and method from body fluid example |
| CN101780396B (en) * | 2010-02-02 | 2012-10-10 | 中国地质大学（武汉） | Absorbing agent of trace organic chloride pesticide in water body and preparation method thereof |
| CN103611334A (en) * | 2013-10-22 | 2014-03-05 | 上海安谱科学仪器有限公司 | Filling method for diatomite column |
| CN103611334B (en) * | 2013-10-22 | 2016-07-06 | 上海安谱实验科技股份有限公司 | A kind of packing method of siliceous earth column |
| CN104667898A (en) * | 2015-02-06 | 2015-06-03 | 玉林师范学院 | Preparation method of eucalyptus-based porous carbon-silicon dioxide solid-phase extraction column |
| CN104667898B (en) * | 2015-02-06 | 2018-12-25 | 玉林师范学院 | A kind of preparation method of eucalyptus base porous carbon-Silica solid phase extraction column |
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| CN1221299C (en) | 2005-10-05 |
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