CN104034817A - Ion chromatography on-line pretreatment for measuring glyphosate in genetically modified soybean oil - Google Patents
Ion chromatography on-line pretreatment for measuring glyphosate in genetically modified soybean oil Download PDFInfo
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- CN104034817A CN104034817A CN201410275486.XA CN201410275486A CN104034817A CN 104034817 A CN104034817 A CN 104034817A CN 201410275486 A CN201410275486 A CN 201410275486A CN 104034817 A CN104034817 A CN 104034817A
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- 239000005562 Glyphosate Substances 0.000 title claims abstract description 41
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 41
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 235000012424 soybean oil Nutrition 0.000 title claims abstract description 23
- 239000003549 soybean oil Substances 0.000 title claims abstract description 23
- 238000004255 ion exchange chromatography Methods 0.000 title claims 5
- 238000000034 method Methods 0.000 claims abstract description 43
- 150000002500 ions Chemical class 0.000 claims abstract description 34
- 150000001450 anions Chemical class 0.000 claims abstract description 14
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 7
- 230000014759 maintenance of location Effects 0.000 claims abstract description 6
- 239000005416 organic matter Substances 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 230000009261 transgenic effect Effects 0.000 claims abstract description 6
- 239000003480 eluent Substances 0.000 claims abstract 2
- 238000000926 separation method Methods 0.000 claims description 18
- 238000005349 anion exchange Methods 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 4
- -1 glyphosate ion Chemical class 0.000 claims description 3
- 230000007246 mechanism Effects 0.000 claims description 3
- 239000000523 sample Substances 0.000 claims 4
- 238000005259 measurement Methods 0.000 claims 1
- 239000012488 sample solution Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 19
- 238000002203 pretreatment Methods 0.000 abstract description 13
- 239000011159 matrix material Substances 0.000 abstract description 5
- 230000000717 retained effect Effects 0.000 abstract description 4
- 239000000575 pesticide Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 11
- 235000010469 Glycine max Nutrition 0.000 description 10
- 244000068988 Glycine max Species 0.000 description 10
- 238000004587 chromatography analysis Methods 0.000 description 8
- 238000001802 infusion Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000002699 waste material Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N acetonitrile Substances CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
- 235000013305 food Nutrition 0.000 description 3
- 230000002363 herbicidal effect Effects 0.000 description 3
- 239000004009 herbicide Substances 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
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- 238000002137 ultrasound extraction Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 230000036541 health Effects 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
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- 108010079442 Anion Transport Proteins Proteins 0.000 description 1
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- 231100000315 carcinogenic Toxicity 0.000 description 1
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- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000021393 food security Nutrition 0.000 description 1
- 235000003869 genetically modified organism Nutrition 0.000 description 1
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- 230000001172 regenerating effect Effects 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
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Abstract
本发明公开了一种离子色谱在线前处理测定转基因大豆油中的草甘膦，先将一定体积的待测样品与水以一定比例混合，超声萃取，使其中的草甘膦溶于水中，后进样用高效液相色谱反相柱在线除去水溶性有机物基质，无保留作用的离子被紧随其后的富集柱保留，柱切换后经淋洗液洗脱的离子在阴离子色谱柱中得到分离，并由抑制电导法进行检测。本发明对在线前处理系统的应用，去除转基因大豆油样品中的水溶性有机物，大豆油中草甘膦农药含量的测定具有广泛深远的意义，本方法改变现有前处理除有机物使用一次性C18柱的状态，减少了人力消耗，节省了样品前处理的时间和繁复的操作过程。
The invention discloses an ion chromatographic on-line pretreatment method for measuring glyphosate in transgenic soybean oil. First, a certain volume of a sample to be tested is mixed with water in a certain proportion, and ultrasonically extracted to dissolve the glyphosate in water, and then the sample is injected. Use high performance liquid chromatography reversed-phase column to remove the water-soluble organic matrix on-line, and the ions without retention are retained by the enrichment column that follows, and the ions eluted by the eluent after column switching are separated in the anion chromatographic column. And detected by inhibited conductometric method. The application of the present invention to the online pretreatment system removes water-soluble organic matter in transgenic soybean oil samples, and the determination of glyphosate pesticide content in soybean oil has extensive and far-reaching significance. The state of the column reduces the labor consumption, saves the time of sample pretreatment and complicated operation process.
Description
Technical field
The present invention relates to a kind of ion chromatographic column switched system, specifically, is that a kind of ion chromatographic column that utilizes switches the new method that the glyphosate in genetically engineered soybean oil is measured in the online pre-treatment of method.
Background technology
Enetically modified food is that some biological gene is utilized modern molecular biology technique to transfer in other species or take the food that genetically modified organism forms as Raw material processing.In order to meet the needs that people are different, transgenic technology makes target species change at aspects such as nutritional quality, shapes, has improved the consumption quality of biologics by transforming biological inhereditary material.About superiority and the potential safety hazard that may exist and the spinoff of enetically modified food, obtained in recent years paying close attention to widely, caused many thinkings.
Resistance glyphosate genetically engineered soybean is that in all genetically modified plants, cultivated area is maximum, a kind of crop that output is maximum, and China is as the maximum Soybean import Guo He country of consumption in the whole world, and the edible overwhelming majority is resistance glyphosate genetically engineered soybean [1] at present.Whether genetically engineered soybean itself there is the reduction of nutritive value and more serious teratogenesis, the check that carcinogenic, mutagenicity is waited until the time.We can predict the impact of resistance glyphosate genetically engineered soybean on health, except deriving from the gene proceeding to, also can derive from the herbicide of generally using in planting process--glyphosate.
Glyphosate is a kind of non-selective, noresidue steriland herbicide, can effectively remove prennical root weeds, is the herbicide [2] being most widely used in the world.Have before this many research to show, the glyphosate of extremely low concentration can promote growth of cancer cells, has stronger carcinogenesis.
Soya-bean oil is the topmost a kind of consumption pattern of soybean, closely bound up with our life, and the residue problem of therefore measuring glyphosate agricultural chemicals in resistance glyphosate genetically engineered soybean oil becomes the problem that people are very deeply concerned.Chromatography of ions is as a kind of the most frequently used technology [3-4] of zwitterion of measuring in aqueous solution, organism because of a large amount of existence in soybean oil in application process produce bottleneck, this method utilize NG1 reverse-phase chromatographic column remove online organism in soya-bean oil and with chromatography of ions coupling, measure glyphosate agricultural chemicals wherein, method is simple, workable, detectability is low.
List of references
The research of glyphosate content in 1 high performance liquid chromatography and ion-chromatographic determination genetically engineered soybean, Zhang Shuo, 2012
2Handbook?of?Chemical?Products-Agricultural?Chemical,Chemical?Industry?Press?of?China,1996,p.363
3H.Small,T.S.Stevens,W.S.Bauman,Novel?ion?exchange?chromatographic?method?using?conductimetric?detection,Anal.Chem.,47(1975)1801-1809
4P.E.Jackson,C.A.Pohl,Advances?in?stationary?phase?development?in?suppressed?ion?chromatography,Trends?Anal.Chem.,16(1997)393-400
Summary of the invention
The object of the invention is to further improve on existing detection method basis, can remove online the water soluble organic substance matrix in sample, utilize anion-exchange column to complete the separation to glyphosate simultaneously, method has the collectivity of height.Institute's use instrument and equipment is simple, highly sensitive, can be widely used in each fields such as environmental monitoring, food security, health and epidemic prevention.
The present invention is achieved by the following technical solutions:
A kind of ion chromatographic column switches the method that glyphosate in genetically engineered soybean oil is measured in the online pre-treatment of method, described system comprises injector, six-way valve, reversed-phase column, ten-way valve, enriching column, anion separation column, four source gradient pumps, infusion pump, electric conductivity detector, waste liquid bottle, injector is connected with six-way valve, six-way valve is connected with reversed-phase column with four source gradient pumps respectively, on ten-way valve, connect enriching column, ten-way valve respectively with infusion pump, anion separation column connects, and connects successively rejector, electric conductivity detector and waste liquid bottle after described anion separation column.
This ion chromatographic column switches the method that glyphosate in genetically engineered soybean oil is measured in the online pre-treatment of method, first the testing sample of certain volume is mixed with certain proportion with water, ultrasonic extraction, make glyphosate wherein soluble in water, rear sample introduction is removed water soluble organic substance matrix online with high performance liquid chromatography reversed-phase column, the ion acting on is without reserve retained by enriching column following closely, and the ion that post switches by leacheate wash-out obtains separation in anion chromatographic column, and detects by suppressing conductance method.
As improving further, the present invention connects high performance liquid chromatography reversed-phase column with anion-exchange column, utilize reversed-phase column organic retention characteristic to be removed to the water soluble organic substance existing in sample, the rear different reserve capability of anion-exchange column to different ions of utilizing, by ion isolation wash-out to be measured, by inhibition conductance method, detect, realized organic online removal in sample, saved the time of sample pre-treatments and complicated operating process.
Described method is applied to measure the glyphosate ion in complex mechanism system, with similar scheme analysis, can improves sensitivity and improve detectability.
Beneficial effect of the present invention is as follows:
The application of the present invention to online preprocessing system, remove the water soluble organic substance in genetically engineered soybean oil samples, in soybean oil, the mensuration of glyphosate pesticide concentration has extensive profound significance, chromatography of ions is as a kind of conventional means of measuring effects of ion, but because a large amount of organism that exist in soya-bean oil are stepped back, this method changes the state that existing pre-treatment organic matter removal is used disposable C18 post, reduced manpower consumption, the time of sample pre-treatments and complicated operating process have been saved, the activating and regenerating of NG1 is processed, compared with the disposable operating characteristic of C18 pillar also more environmental protection, there is no in addition this type of detection method both at home and abroad.
Accompanying drawing explanation
Fig. 1 is structure and the work schematic diagram that the glyphosate in genetically engineered soybean oil is measured in the online pre-treatment of chromatography of ions of the present invention;
In Fig. 1,1-injector; 2-six-way valve; 3-reversed-phase column; 4-enriching column; 5-ten-way valve; 6-anion separation column; 7-four source gradient pumps; 8-NaOH leacheate; 9-infusion pump; 10-electric conductivity detector; 11-acetonitrile; 12-water; 13-waste liquid bottle;
Glyphosate assay and add target chromatogram in Fig. 2 genetically engineered soybean oil;
In Fig. 2, a-actual sample chromatogram, b-actual sample mark-on 0.2mg/L glyphosate chromatogram, the chromatographic peak of 1-glyphosate in this method system.
Embodiment
The invention discloses a kind of ion chromatographic column and switch the method that glyphosate in genetically engineered soybean oil is measured in the online pre-treatment of method, system comprises injector 1, six-way valve 2, reversed-phase column 3, ten-way valve 5, enriching column 4, anion separation column 6, four source gradient pumps 7, infusion pump 9, electric conductivity detector 10, waste liquid bottle 13, injector 1 is connected with six-way valve 2, six-way valve 2 is connected with reversed-phase column 3 with four source gradient pumps 7 respectively, on ten-way valve 5, connect enriching column 4, ten-way valve 5 respectively with infusion pump 9, anion separation column 6 connects, after described anion separation column 6, connect successively rejector, electric conductivity detector 10 and waste liquid bottle 13.
This ion chromatographic column switches the method that glyphosate in genetically engineered soybean oil is measured in the online pre-treatment of method, first the testing sample of certain volume is mixed with certain proportion with water, ultrasonic extraction, make glyphosate wherein soluble in water, rear sample introduction is removed water soluble organic substance matrix online with high performance liquid chromatography reversed-phase column 3, the ion acting on is without reserve retained by enriching column 4 following closely, the ion that post switches by leacheate wash-out obtains separation in anion separation column 6, and detects by suppressing conductance method.
The present invention connects high performance liquid chromatography reversed-phase column 3 with anion separation column 6, utilize 3 pairs of organic retention characteristics of reversed-phase column to remove the water soluble organic substance existing in sample, the rear different reserve capability of utilizing 6 pairs of different ions of anion separation column, by ion isolation wash-out to be measured, by inhibition conductance method, detect, realized organic online removal in sample, saved the time of sample pre-treatments and complicated operating process.
Described method is applied to measure the glyphosate ion in complex mechanism system, with similar scheme analysis, can improves sensitivity and improve detectability.
Below by specific embodiment, in conjunction with Figure of description, technical scheme of the present invention is described in further detail:
The invention provides a kind of new analytical approach of measuring glyphosate in genetically engineered soybean oil, utilize an ICS-2100 ion chromatograph to comprise a six-way valve 2, an infusion pump 9, ten-way valve 5, electric conductivity detector 10, take IonPacAS11-HC as anion-exchange column 6, pre-treatment post 3 be take water as mobile phase, flow velocity is 1.0mL/min, chromatographically pure acetonitrile 11 is regenerated liquid, 0.5mL/min, analytical column leacheate mobile phase is 23mmol/LNaOH, flow velocity is 1.0mL/min, sample size is 100 μ L, it is 52mA that rejector suppresses electric current, electric conductivity detector 10 detects.
The present invention utilizes reversed-phase column 3 to remove online the water soluble organic substance matrix in sample, the separated glyphosate of anion-exchange column 6, suppressing conductance method detects, installation drawing as shown in Figure 1, system comprises injector 1, six-way valve 2, reversed-phase column 3, enriching column 4, ten-way valve 5, anion separation column 6, four source gradient pumps 7, infusion pump 9, electric conductivity detector 10, waste liquid bottle 13, injector 1 is connected with six-way valve 2, six-way valve 2 is connected with reversed-phase column 3 with four source gradient pumps 7 respectively, on ten-way valve 5, connect enriching column 4, ten-way valve 5 respectively with infusion pump 9, anion separation column 6 connects, after described anion separation column, connect successively electric conductivity detector 10 and waste liquid bottle 13.
Fig. 1 is structure and the work schematic diagram that the online pretreatment technology of chromatography of ions is measured the glyphosate in genetically engineered soybean oil.Concrete implementation step is: by four source gradient pumps 7, by the sample that is full of quantitative ring (100 μ L) under water (flow velocity is 1mL/min) is carried, the online water soluble organic substance of removing in reversed-phase column 3, solution through wash-out is retained in enriching column, after 2min, transfer valve 5, the measured ion for the treatment of in enriching column 4 is transported to separated wash-out in anion-exchange column 6, adopts inhibition conductance method to detect, and peak area method is quantitative.
Fig. 2 is the chromatogram that the online pretreatment technology of chromatography of ions is measured the glyphosate in genetically engineered soybean oil.Pre-treating method, for pipetting soybean oil 5mL to be determined, adds 5mL deionized water, and in ultrasonic cell disrupte instrument, the about 20min of ultrasonic extraction, fully mixes it, and the centrifugal 15min of rotating speed 12000r/min collects lower floor's water and filters through 0.22 μ m nylon leaching film, stand-by.By figure, be not difficult to find, this method does not measure glyphosate in actual sample, by mark-on experiment, can be found out, after the separation of ion chromatographic column, other ions that exist in oil can not disturb the mensuration of glyphosate, and while method has high sensitivity, and method is reliable, practical advantage.
Finally, it is also to be noted that, what more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (4)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424865A (en) * | 2015-12-10 | 2016-03-23 | 苏州国环环境检测有限公司 | Illegal cooking oil detection method |
| CN105548413A (en) * | 2015-12-10 | 2016-05-04 | 苏州国环环境检测有限公司 | Method for pre-treating gutter-oil detection sample |
| CN105929033A (en) * | 2016-04-12 | 2016-09-07 | 海南大学 | System and method for measuring trace lactic acid ion in lobaplatin by using column switching-ion chromatography method |
| CN110187035A (en) * | 2019-07-02 | 2019-08-30 | 北京市水文总站 | The analyzing detecting method of Drinking Water glyphosate |
| CN110988243A (en) * | 2019-12-23 | 2020-04-10 | 天津量信检验认证技术有限公司 | Ion chromatography-mass spectrometry detection method for glyphosate content in fruits |
| CN113156041A (en) * | 2020-12-28 | 2021-07-23 | 吉林省生态环境监测中心 | Detection method of glyphosate |
| CN114740112A (en) * | 2022-04-06 | 2022-07-12 | 浙江省林业科学研究院 | Method for extracting and purifying glyphosate residual quantity in vegetable oil |
-
2014
- 2014-06-19 CN CN201410275486.XA patent/CN104034817A/en active Pending
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424865A (en) * | 2015-12-10 | 2016-03-23 | 苏州国环环境检测有限公司 | Illegal cooking oil detection method |
| CN105548413A (en) * | 2015-12-10 | 2016-05-04 | 苏州国环环境检测有限公司 | Method for pre-treating gutter-oil detection sample |
| CN105929033A (en) * | 2016-04-12 | 2016-09-07 | 海南大学 | System and method for measuring trace lactic acid ion in lobaplatin by using column switching-ion chromatography method |
| CN110187035A (en) * | 2019-07-02 | 2019-08-30 | 北京市水文总站 | The analyzing detecting method of Drinking Water glyphosate |
| CN110988243A (en) * | 2019-12-23 | 2020-04-10 | 天津量信检验认证技术有限公司 | Ion chromatography-mass spectrometry detection method for glyphosate content in fruits |
| CN113156041A (en) * | 2020-12-28 | 2021-07-23 | 吉林省生态环境监测中心 | Detection method of glyphosate |
| CN114740112A (en) * | 2022-04-06 | 2022-07-12 | 浙江省林业科学研究院 | Method for extracting and purifying glyphosate residual quantity in vegetable oil |
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Application publication date: 20140910 |