CN102384948A - Method for measuring dicyandiamide in fertilizer and fertilizer additives - Google Patents
Method for measuring dicyandiamide in fertilizer and fertilizer additives Download PDFInfo
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- CN102384948A CN102384948A CN2011102201016A CN201110220101A CN102384948A CN 102384948 A CN102384948 A CN 102384948A CN 2011102201016 A CN2011102201016 A CN 2011102201016A CN 201110220101 A CN201110220101 A CN 201110220101A CN 102384948 A CN102384948 A CN 102384948A
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Abstract
A kind of measuring method for dicyandiamide in fertilizer and fertilizer additive,It is characterized by comprising following steps: get dicyandiamide standard solution ready,And sample pre-treatments: wherein sample pre-treatments, which refer to, weighs quantitative sample,The ultrapure water of 2 times of volumes is added,After ultrasonic extraction centrifugation,Supernatant obtains sample filtrate after being filtered,Add water constant volume; Sample measurement: sample filtrate and the dicyandiamide standard solution got ready are injected in high performance liquid chromatography,Dicyandiamide in standard solution and sample, which is measured, according to chromatographic condition absorbs peak area; As a result it calculates: by the linear relationship curve of the concentration of dicyandiamide standard solution and corresponding absorption peak area,The concentration of dicyandiamide in sample filtrate is checked in,According to
Formula calculates the content of dicyandiamide in sample. The invention has the advantages that method is quick, easy; Detection limits low (0.1mg/kg); Rate of recovery height (91.27%~98.48%).
Description
One, technical field
The present invention relates to the method that a kind of (High performance liquid chromatography) detects dicyandiamide content, particularly a kind of assay method (highly effective liquid phase chromatography detection method) that is used for fertilizer and fertilizer additive dicyandiamide.
Two, background technology
Dicyandiamide (DCD) is also referred to as dicyanodiamine, is a kind of by generally acknowledged nitrification inhibitor of high quality and at a reasonable price, is one of nitrification inhibitor few in number that in production reality, is applied.The reported first dicyandiamide had the inhibiting nitrification characteristic in 1918; The 1970s and 1980s in last century, the U.S. began on agricultural, to apply as a kind of nitrification inhibitor commodity it; Preceding West Germany SKW company utilizes dicyandiamide to register the nitrification inhibitor product of commodity Didin by name; Scientific research institutions and part fertilizer production enterprises such as domestic Shenyang Inst. of Applied Ecology, Chinese Academy of Sciences also all utilize dicyandiamide to produce products such as long-acting new-type fertilizer, stable fertilizer, fertilizer synergist.Current dicyandiamide is widely used in the production of slow release fertilizer or fertilizer additive at home and abroad, and series of products receive the concern of countries in the world, especially on the market of China, US and European.
Dicyandiamide is in the production run of fertilizer or fertilizer additive, and part will be decomposed generation ammonia (the dicyandiamide WS was prone to decompose in time more than 80 ℃), will affect the content of dicyandiamide in fertilizer or the fertilizer additive finished product, thereby influence its effect.The application of farmland dicyandiamide; An amount of dicyandiamide of most result of study support is to the conclusion (dicyandiamide is degraded about 70 days in soil) of environment and crop nonhazardous effect; But also there are some researches show; Dicyandiamide is prone to the water leaching loss, uses when improper or excessive, crop is caused poison even residual in agricultural product easily.The dicyandiamide what state of in fertilizer or fertilizer additive processing, degrading; Containing the fertilizer of dicyandiamide or the dicyandiamide leaching loss in fertilizer additive entering water body is that human body sucks, and the agricultural residual human health that whether can influence for human body is edible that excessive dicyandiamide causes does not still have definite report at present.
The little poison of dicyandiamide or nontoxic basically, acute toxicity is very little, and in pharmaceutical production, dicyandiamide is processed intermedium as medicine, is detection necessary in the domestic and international medicine finished product.Dicyandiamide is as the dimer of cyanamide, and it is similar to mouse poisoning symptom and cyanamide tripolymer melamine, and consistent poisoning symptom appears in the mouse after the dicyandiamide of 13000mg/kg dosage and the melamine administration; All occur uneasy; Jump, be short of breath, just dead in dozens of minutes subsequently.Contain the fertilizer of dicyandiamide or fertilizer additive is long-term or excessive using, it is unknown at present whether dicyandiamide wherein can become a kind of potential hazardous agents as melamine.Therefore; Though leaching loss and the residual phenomenon of farming that fertilizer that using of not finding as yet at present to occur in the agricultural production contains dicyandiamide or fertilizer additive cause, however, in view of the necessary detection of dicyandiamide as medicine; With and have a mouse poisoning symptom similar with melamine; Scientific research personnel and production application person are necessary to monitor the dicyandiamide that is widely used in fertilizer or the fertilizer additive production, and the actual content of clear and definite dicyandiamide is prevented trouble before it happens.
Present domestic High performance liquid chromatography is to the mensuration of dicyandiamide; All concentrate on detection to impurity dicyandiamide in medicine example hydrochloric acid diformin tablet, the DB2 etc.; Wherein dicyandiamide mainly is to use as medicine processing intermedium, and detection method is measured dicyandiamide content with reference to the method in the version Pharmacopoeia of the People's Republic of China in 2005 or the method for revision mostly.The weak point of these methods is that the chromatographic column price is higher, the life-span short, and the retention time of dicyandiamide peak (peak value) is shorter during chromatographic resolution; Be difficult to and the solvent peak baseline separation; Specificity is strong inadequately, and the chromatographic condition reappearance is not good enough, and detectability is higher; Detection sensitivity is lower, and the detection that is difficult to satisfy micro-dicyandiamide requires or the like.In addition, more crucial is uses wherein that the chromatographic condition of some method detects the dicyandiamide content in the fertilizer, fails well the assorted peak of dicyandiamide chromatographic peak and other to be separated.China still lacks as the monitoring that nitrification inhibitor is added into one of fertilizer or as fertilizer sources additive component dicyandiamide at present; I.e. detection to dicyandiamide content in fertilizer or the fertilizer additive still lacks; Therefore; The necessary actual conditions that combine China are explored a kind of detection method that is suitable for dicyandiamide in fertilizer and the fertilizer additive.
Three, summary of the invention
The purpose of this invention is to provide a kind of assay method (highly effective liquid phase chromatography detection method) that is used for fertilizer and fertilizer additive dicyandiamide, making becomes that a kind of detectability is low, detection sensitivity is high, the recovery is high and highly effective liquid phase chromatography detection method fast.
Of the present invention opening one's minds is: adopt high performance liquid chromatography when dicyandiamide content detects in fertilizer and the fertilizer additive; All need grope and seek suitable chromatographic condition, comprise chromatographic column, moving phase, flow velocity, sampling volume, column temperature, post pressure, detect wavelength etc.In addition, also need confirm the detection method that a cover and method for distilling are complementary, these all are directly connected to the recovery, accuracy and the sensitivity of extraction and detection method.So to achieve these goals, the present invention need explore and set up a kind of extraction conditions of dicyandiamide in fertilizer and the fertilizer additive and new chromatographic condition of being applicable to.
In view of more than open one's minds; A kind of assay method that is used for fertilizer and fertilizer additive dicyandiamide provided by the present invention is characterized in that this assay method comprises the steps: 1. to get ready the dicyandiamide standard solution, and sample pre-treatments: wherein sample pre-treatments is meant and takes by weighing quantified sample (comprising fertilizer sample and/or fertilizer additive sample); The ultrapure water that adds 2 times of volumes; After ultrasonic Extraction was centrifugal, supernatant obtained sample filtrating after filtrator filters, add the water constant volume; 2. sample determination: sample filtrating and the dicyandiamide standard solution got ready are injected high performance liquid chromatography respectively, according to dicyandiamide absorption peak area in chromatographic condition bioassay standard solution and the sample; 3. the result calculates: through the concentration of dicyandiamide standard solution and the linear relationship curve of corresponding absorption peak area; Check in the concentration of dicyandiamide in the sample filtrating, according to the content of dicyandiamide in
formula calculation sample.
In the formula:
The massfraction of dicyandiamide in the W-sample, mg/kg;
C-is by the concentration of dicyandiamide in the appearance liquid of finding on the typical curve, ug/mL;
The final constant volume of V-appearance liquid, mL;
Ts-obtains multiple;
M-sample mass (oven dry appearance quality), g.
Above-mentioned sample preparation is for accurately taking by weighing fertilizer or the fertilizer additive sample of 10.000-20.000g; The ultrapure water that adds 40mL, ultrasonic Extraction 30min, the centrifugal 10min of extract 4000r/min; Supernatant filters with the needle-based filtrator of 0.45um, is settled to 50mL after the filtration.
Above-mentioned dicyandiamide standard solution preparation is settled to 100ml for accurately taking by weighing 0.001g dicyandiamide AR with ultrapure water, gets C
Mark=100ug/mL places 4 ℃ of refrigerators to preserve.
The above-mentioned instrument that uses is Waters Alliance 2695 PDADs, chromatographic condition be chromatographic column adopting Waters XTerra RP-18 (4.6mm * 150mm, 5um); Mobile phase A is an acetonitrile, and Mobile phase B is 4-butyl ammonium hydrogen sulfate ((C
4H
9)
4NHSO
4) and sodium dihydrogen phosphate (NaH
2PO
4) mixed liquor, the volume ratio of mobile phase A and Mobile phase B is (mobile phase A: Mobile phase B is) 5: 95, and flow velocity is 0.7000mL/min, and sampling volume is 10uL; Column temperature is 30 ℃, and post is pressed and is 14Mpa, and the ultraviolet detection wavelength is 220nm.
Above-mentioned high performance liquid chromatography has a single-minded chromatographic peak at 2.60--3.30min, and this peak is consistent with the chromatographic peak in the standard solution, is the characteristic absorption peak of dicyandiamide.
Because it mainly is the mensuration to impurity dicyandiamide in the medicine that present domestic High performance liquid chromatography is measured dicyandiamide; Measure dicyandiamide content in fertilizer material and the fertilizer additive if use specimen preparation, chromatographic condition and the detection wavelength of prior art; Other material possibly have overlappingly with the dicyandiamide chromatographic peak, can not accurately detect dicyandiamide content.
Compared with prior art; The present invention has the following advantages: the present invention is applicable to dicyandiamide Determination on content in fertilizer and the fertilizer additive; And do not receive the interference at other assorted peak, this method fast (method simple, be prone to row), highly sensitive (precision of detection is high), detectability is low, the recovery is high.Use dicyandiamide content in high effective liquid chromatography for measuring fertilizer of the present invention and the fertilizer additive, the solid sample detection of extracting after filtering is limited to 0.1mg/kg, and the recovery is 91.27%～98.48%.
Four, description of drawings
Fig. 1 is dicyandiamide standard items chromatograms;
Fig. 2 is a kind of slow-release compound fertilizer sample chromatogram figure that contains dicyandiamide;
Fig. 3 is a kind of fertilizer additive sample chromatogram figure that contains dicyandiamide.
Five, embodiment
Utilize high performance liquid chromatography that the content of dicyandiamide in a kind of slow release fertilizer and the fertilizer additive is detected:
1, instrument and equipment
Waters Alliance 2695 high performance liquid chromatographs are furnished with Waters 2996 PDADs.
2, select reagent for use
Acetonitrile (chromatographically pure);
4-butyl ammonium hydrogen sulfate (2mmol/L): accurately take by weighing 0.679g 4-butyl ammonium hydrogen sulfate AR, be settled to 1000ml with ultrapure water;
Sodium dihydrogen phosphate (25mmol/L): accurately take by weighing 3.000g sodium dihydrogen phosphate AR, be settled to 1000ml with ultrapure water;
Dicyandiamide titer: accurately take by weighing 0.001g dicyandiamide AR, be settled to 100ml, get C with ultrapure water
Mark=100ug/mL places 4 ℃ of refrigerators to preserve.
3, operation steps
1. sample preparation: the slow release fertilizer or the fertilizer additive that accurately take by weighing 10.000--20.000g; Add a certain amount of ultrapure water; Ultrasonic Extraction 30min, the centrifugal 10min of extract 4000r/min, supernatant filters with the needle-based filtrator of 0.45um; Be settled to 50mL after the filtration, supply high-performance liquid chromatogram determination.
2. sample determination: with the dicyandiamide standard solution, sample filtrating is injected high performance liquid chromatography, according to dicyandiamide absorption peak area in chromatographic condition bioassay standard solution and the sample.Chromatographic condition be chromatographic column adopting Waters XTerra RP--18 (4.6mm * 150mm, 5um); Mobile phase A is an acetonitrile, and Mobile phase B is 4-butyl ammonium hydrogen sulfate ((C
4H
9)
4NHSO
4) and sodium dihydrogen phosphate (NaH
2PO
4) mixed liquor, (mobile phase A: Mobile phase B) be 5: 95, flow velocity is 0.7000mL/min to the volume ratio of mobile phase A and Mobile phase B, and sampling volume is 10uL; Column temperature is 30 ℃, and post is pressed and is 14Mpa, and the ultraviolet detection wavelength is 220nm.
3. the drafting of typical curve: use moving phase dicyandiamide standard reserving solution stepwise dilution to be obtained concentration is 1,10,25,50,75, the standard industry liquid of 100ug/mL; Concentration is sample detection from low to high; With peak area-concentration mapping, obtain the typical curve regression equation.
Dicyandiamide concentration is in 1～100ug/mL scope, and the concentration peak area value corresponding with it is the good linear relation, and related coefficient is 0.999.The gained linear equation is: (x is a concentration to y=134445x-102557, ug/mL; Y is a peak area, uvs)
4, the result calculates
Calculate by following formula:
In the formula:
The massfraction of dicyandiamide in the W-sample, mg/kg;
C-is by the concentration of dicyandiamide in the appearance liquid of finding on the typical curve, ug/mL;
The final constant volume of V-appearance liquid, mL;
Ts-obtains multiple;
M-sample mass (oven dry appearance quality), g.
The solid sample that calculates with 3 times of signal to noise ratio (S/N ratio)s (S/N) detects and is limited to 0.1mg/kg, and the solid sample that calculates with 10 times of signal to noise ratio (S/N ratio)s (S/N) quantitatively is limited to 0.33mg/kg.
5, the recovery
Set 3 additions, with dicyandiamide and the abundant mixing of fertilizer sample, to each addition replication 6 times.
Table 1 fertilizer adds the recovery of dicyandiamide
6, actual sample analysis (reaching the detection of dicyandiamide in certain fertilizer additive sample in certain slow-release compound fertilizer sample)
The dicyandiamide standard model has a single absorption peak (see figure 1) at 220nm wavelength sample introduction 2.60～3.30min; Use this method can detect in the special-purpose fertilizer of a certain long-acting slow-release tealeaves and a certain long-acting sustained-release complex fertilizer adjuvant NAM in dicyandiamide do not have assorted peak and disturb; 2.60～3.30min has a single dicyandiamide absorption peak; Dicyandiamide content in calculating special-purpose fertilizer of long-acting slow-release tealeaves and long-acting sustained-release complex fertilizer adjuvant NAM is respectively 565mg/kg and 42g/kg (seeing Fig. 2,3).
Above embodiment only is a preferred implementation of the present invention, is not that scope of the present invention is limited, and protection scope of the present invention should be as the criterion with claim institute restricted portion, is applicable to fertilizer and fertilizer additive that all contain dicyandiamide.For those skilled in the art, do not breaking away from the spirit and scope of the present invention, can also make some improvement and retouching, these improvement and retouching also should be regarded as the protection domain that claims of the present invention are confirmed.
Claims (5)
1. assay method that is used for fertilizer and fertilizer additive dicyandiamide; It is characterized in that comprising the steps: 1. getting ready the dicyandiamide standard solution; And sample pre-treatments: wherein sample pre-treatments is meant and takes by weighing quantified sample, adds the ultrapure water of 2 times of volumes, after ultrasonic Extraction is centrifugal; Supernatant obtains sample filtrating after filtrator filters, add the water constant volume; 2. sample determination: sample filtrating and the dicyandiamide standard solution got ready are injected high performance liquid chromatography, according to dicyandiamide absorption peak area in chromatographic condition bioassay standard solution and the sample; 3. the result calculates: through the concentration of dicyandiamide standard solution and the linear relationship curve of corresponding absorption peak area; Check in the concentration of dicyandiamide in the sample filtrating, according to the content of dicyandiamide in
formula calculation sample;
In the formula:
The massfraction of dicyandiamide in the W-sample, mg/kg;
C-is by the concentration of dicyandiamide in the appearance liquid of finding on the typical curve, ug/mL;
The final constant volume of V-appearance liquid, mL;
Ts-obtains multiple;
M-sample mass (oven dry appearance), g.
2. the assay method that is used for fertilizer and fertilizer additive dicyandiamide according to claim 1; It is characterized in that: above-mentioned sample preparation is: the new-type fertilizer or the fertilizer additive that accurately take by weighing 10.000-20.000g; The ultrapure water that adds 40mL, ultrasonic Extraction 30min, the centrifugal 10min of extract 4000r/min; Supernatant filters with the needle-based filtrator of 0.45um, is settled to 50mL after the filtration.
3. the assay method that is used for fertilizer and fertilizer additive dicyandiamide according to claim 1 is characterized in that: above-mentioned dicyandiamide standard solution preparation is: accurately take by weighing 0.001g dicyandiamide AR, be settled to 100ml with ultrapure water, get C
Mark=100ug/mL preserves in 4 ℃ of refrigerators.
4. the assay method that is used for fertilizer and fertilizer additive dicyandiamide according to claim 1; It is characterized in that: the above-mentioned instrument that uses is Waters Alliance 2695 PDADs; Chromatographic condition is: and chromatographic column adopting WatersXTerra RP-18 (4.6mm * 150mm, 5um); Mobile phase A is an acetonitrile, and Mobile phase B is 4-butyl ammonium hydrogen sulfate ((C
4H
9)
4NHSO
4) and sodium dihydrogen phosphate (NaH
2PO
4) mixed liquor, (mobile phase A: Mobile phase B) be 5: 95, flow velocity is 0.7000mL/min to the volume ratio of moving stream phase A and Mobile phase B, and sampling volume is 10uL; Column temperature is 30 ℃, and post is pressed and is 14Mpa, and the ultraviolet detection wavelength is 220nm.
5. the assay method that is used for fertilizer and fertilizer additive dicyandiamide according to claim 1; It is characterized in that: above-mentioned high performance liquid chromatography has a single-minded chromatographic peak at 2.60-3.30min; This peak is consistent with the chromatographic peak in the standard solution, is the characteristic absorption peak of dicyandiamide.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103344726A (en) * | 2013-06-14 | 2013-10-09 | 中华人民共和国温州出入境检验检疫局 | Method for extraction of dicyandiamide component in dairy product |
| CN104502473A (en) * | 2014-12-10 | 2015-04-08 | 黄河三角洲京博化工研究院有限公司 | Quantitative method of detecting cyanamide by utilizing HPLC method |
| CN107561203A (en) * | 2016-06-30 | 2018-01-09 | 吉林贝盈生物科技有限公司 | The detection method of dicyandiamide content in a kind of fertilizer |
| CN108195986A (en) * | 2018-01-15 | 2018-06-22 | 黄河三角洲京博化工研究院有限公司 | A kind of method of urea, dicyandiamide, content of melamine in LC-MS analysis guanidine hydrochloride and its three wastes |
| CN110618227A (en) * | 2019-10-17 | 2019-12-27 | 北京君德同创生物技术股份有限公司 | Method for detecting dicyandiamide content in cyanamide solution by using HPLC method |
-
2011
- 2011-07-28 CN CN2011102201016A patent/CN102384948A/en active Pending
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103344726A (en) * | 2013-06-14 | 2013-10-09 | 中华人民共和国温州出入境检验检疫局 | Method for extraction of dicyandiamide component in dairy product |
| CN104502473A (en) * | 2014-12-10 | 2015-04-08 | 黄河三角洲京博化工研究院有限公司 | Quantitative method of detecting cyanamide by utilizing HPLC method |
| CN107561203A (en) * | 2016-06-30 | 2018-01-09 | 吉林贝盈生物科技有限公司 | The detection method of dicyandiamide content in a kind of fertilizer |
| CN108195986A (en) * | 2018-01-15 | 2018-06-22 | 黄河三角洲京博化工研究院有限公司 | A kind of method of urea, dicyandiamide, content of melamine in LC-MS analysis guanidine hydrochloride and its three wastes |
| CN108195986B (en) * | 2018-01-15 | 2019-11-05 | 黄河三角洲京博化工研究院有限公司 | A kind of method that LC-MS analyzes urea, dicyandiamide, content of melamine in guanidine hydrochloride and its three wastes |
| CN110618227A (en) * | 2019-10-17 | 2019-12-27 | 北京君德同创生物技术股份有限公司 | Method for detecting dicyandiamide content in cyanamide solution by using HPLC method |
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Application publication date: 20120321 |