CN110187035A - The analyzing detecting method of Drinking Water glyphosate - Google Patents
The analyzing detecting method of Drinking Water glyphosate Download PDFInfo
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Abstract
The present invention relates to a kind of analyzing detecting methods of Drinking Water glyphosate.The present invention provides a kind of analyzing detecting methods of drinking water glyphosate, which is characterized in that the analyzing detecting method includes the following steps: that (1) determines the operating parameter of ion chromatograph；Flow rate of mobile phase is 0.8-1.0mL/min, and chromatographic column used includes AS19 analytical column and AG19 guard column；(2) standard curve of glyphosate is made；And (3) determine the content of sample glyphosate.Method of the present invention is not necessarily to sample pre-treatments, is directly entered instrument and is analyzed；Without post column derivatization; it is easy to operation; using AS19 analytical column and AG19 guard column; increase sample volume; the temperature of column temperature and conductance cell is optimized, so that the present invention has more practicability and generalization, and small using the standard deviation of analyzing detecting method of the present invention; recovery of standard addition is 98.8-101%, is conducive to the detection of batch samples.
Description
Technical field
The present invention relates to the analyzing detecting methods of pesticide index in Drinking Water, are specifically related to a kind of Drinking Water
The analyzing detecting method of glyphosate.
Background technique
Glyphosate is the effective active chemical component in widely used many herbicides, it is received in the use of European Union
Strict supervision.Glyphosate and genetically modified crops have no direct relation, and non-transgenic crop will equally beat herbicide glyphosate.Europe
Continent food safety office (EFSA) and EU member country are completed and reappraise to herbicide glyphosate, they issue report and point out
Glyphosate is very big may carcinogenic risk to the mankind, while it is remaining to also proposed some new food glyphosates that tighten control
Safety measure.On October 27th, 2017, the carcinogenic substance inventory edit that international cancer research institution, the World Health Organization announces
With reference to glyphosate is in 2A class carcinogenic substance inventory.
China, will be careless in " standards for drinking water quality " (GB5749-2006) that on July 1st, 2007 formally executes
Sweet phosphine is classified as the unconventional index of water quality, and provides that its limit value is 0.7mg/L.Simultaneously in " the drinking water standard method of inspection "
(GB5750-2006) in pesticide index fascicle (GB5750.9-2006), corresponding detection method is given.
It is given in " the drinking water standard method of inspection " (GB5750-2006) pesticide index fascicle (GB5750.9-2006)
Detection method out is using high pressure lipuid chromatography (HPLC).This method can obtain lesser relative deviation and higher mark-on returns
Yield.But this method needs to carry out sample the operation of post-column derivation, process is complex and reproducibility and accuracy rate are difficult to
Accurately ensured.The reagent needed in the analysis process simultaneously is more, prepares and operating process is also relatively complicated, be unfavorable for
The analysis detection of batch samples.
Han Wanru (Han Wanru water with ion chromatography glyphosate [J] hydrotechny, 2018,12 (66), 0164-
66.) use Ion PAC AS11-HC (250mm × 4mm) for analytical column, EGC occur online KOH be leacheate, inhibit conductance into
Row detection, carries out quantitative analysis with the peak area of glyphosate.Its chromatographic condition used is that EGC (KOH) leacheate occurs online
The on-line automatic generation 30mmolKOH leacheate of device, with the isocratic elution of the flow velocity of 1.20mL/min, 25 μ L sampling volumes inhibit electricity
Detection is led, 90mA inhibits electric current, and post case temperature is 25 DEG C, and detection cell temperature is 35 DEG C, and the chromatographic run time is 10min, tool
Have the disadvantage that: 1) flow velocity is very fast, will cause instrument pressure rise, and baseline stability is deteriorated, and noise increases；2) sampling volume mistake
It is small: to will cause the quantitative inaccuracy of target to be measured of low content or even can't detect, there are deviation, small sample volumes pair for testing result
Instrument analytical column, suppressor, electric conductivity detector are also relatively high in the requirement of precision aspect, are unfavorable for the popularization and application of method；
3) runing time is shorter: influence sample in each component separating effect, especially in sample to be tested contained ionic species it is more or
When certain constituent contents are excessive, component to be measured can be caused to cover, influence quantitative accuracy.
Summary of the invention
For this purpose, there is provided a kind of analysis detection sides of Drinking Water glyphosate for technical problem solved by the invention
Method, this method do not need any reagent, and step is simple, and accuracy in detection is high.
The present invention provides a kind of analyzing detecting methods of drinking water glyphosate, which is characterized in that the analysis detection
Method includes the following steps:
(1) operating parameter of ion chromatograph is determined；Flow rate of mobile phase is 0.8-1.0mL/min, chromatographic column packet used
Analytical column containing AS19 and AG19 guard column；
(2) standard curve of glyphosate is made；And
(3) content of sample glyphosate is determined.
Specifically, the invention proposes following technical solutions.
The present invention provides a kind of analyzing detecting methods of drinking water glyphosate, which is characterized in that the analysis detection
Method includes the following steps:
(1) operating parameter of ion chromatograph is determined；Flow rate of mobile phase is 0.8-1.0mL/min, chromatographic column packet used
Analytical column containing AS19 and AG19 guard column；
(2) standard curve of glyphosate is made；And
(3) content of sample glyphosate is determined.
Preferably, for analyzing detecting method described above, wherein leacheate is the aqueous slkali of 20-40mmol/L；It is excellent
Choosing, the leacheate is the aqueous slkali of 30mmol/L；More preferably, the aqueous slkali is the molten of sodium hydroxide or potassium hydroxide
Liquid.
Preferably, for analyzing detecting method described above, wherein conductance cell temperature be 25-35 DEG C, preferably 30
℃；And/or
Column temperature is 25-35 DEG C, preferably 30 DEG C；And/or
Sampling volume is 80-120 μ L, preferably 100 μ L；And/or
Inhibition electric current is 80-100mA, preferably 90mA；And/or
Analysis time is 20-40min, preferably 30min.
Preferably, for analyzing detecting method described above, wherein the AS19 analytical column and AG19 guard column it is interior
Diameter is 4nm.
Preferably, for analyzing detecting method described above, wherein the standard curve of production glyphosate in step (2)
Method include the following steps:
1) glyphosate standard reserving solution is prepared；
2) aspiration step 1) in Standard Reserving Solution obtain standard solution with water constant volume；
3) it takes the standard solution of step 2) to be diluted respectively, obtains standard solution；
4) standard solution is analyzed using ion chromatograph, draws standard curve.
Preferably, for analyzing detecting method described above, wherein in step 1), the glyphosate standard reserve
The concentration of liquid is 100-500mg/L, preferably 100mg/L, it is further preferred that the glyphosate standard reserving solution is to have card to mark
Quasi- substance has card standard sample.
Preferably, for analyzing detecting method described above, wherein in step 2), the glyphosate standard is used
The concentration of liquid is 10-50mg/L, preferably 10mg/L.
Preferably, for analyzing detecting method described above, wherein in step 3), the concentration of the standard solution
Respectively 0mg/L, 0.02-0.05mg/L, 0.08-0.10mg/L, 0.15-0.25mg/L, 0.30-0.50mg/L, 0.80-
1.00mg/L and 1.50-2.00mg/L, it is preferred that the concentration of the standard solution solution is 0mg/L, 0.05mg/L, 0.10mg/
L, 0.20mg/L, 0.50mg/L, 1.00mg/L and 2.00mg/L.
Preferably, for analyzing detecting method described above, wherein in step 3), the volume point of standard solution
Not are as follows: 0mL, 0.02-0.05mL, 0.08-0.10mL, 0.15-0.25mL, 0.30-0.50mL, 0.80-1.00mL and 1.50-
2.00mL, it is preferred that the volume of the standard solution be 0mL, 0.05mL, 0.10mL, 0.20mL, 0.50mL, 1.00mL and
2.00mL。
Preferably, for analyzing detecting method described above, wherein carrier gas is nitrogen.
Beneficial effect obtained by the present invention is:
1. the method for the present invention is not necessarily to sample pre-treatments, it is directly entered instrument and is analyzed；Without post column derivatization, operation letter
Easy row.
2. increasing sample volume present invention employs AS19 analytical column and AG19 guard column, column temperature and conductance cell are optimized
Temperature so that the present invention have more practicability and generalization.
3. analytic process of the invention entire carries out automatic sampling to sample, analyzes, provides testing result, analysis time 30
Minute, it has saved time and labour, it is more efficient and convenient.
4. entire analytic process of the invention only needs addition deionized water, without adding other chemical reagent.Operator without
The poisonous and harmful organic solvent of contact need to be contacted, and test sample is convenient, saves manpower and time, is conducive to the analysis of batch samples
Detection.
5. the standard deviation using analyzing detecting method of the present invention is small, recovery of standard addition 98.8-101% has
Conducive to the detection of batch samples.
Detailed description of the invention
Fig. 1 is obtained glyphosate standard working curve schematic diagram in embodiment 1；
Fig. 2 is the chromatography of ions figure of the standard sample in embodiment 1-1；
Fig. 3 is the chromatography of ions figure of the standard sample in comparative example 1；
Fig. 4 is the chromatography of ions figure of the standard sample in comparative example 2；
Fig. 5 is the chromatography of ions figure of the standard sample in comparative example 3；
Fig. 6 is the chromatography of ions figure of the standard sample in comparative example 4；
Fig. 7 is the chromatography of ions figure of the standard sample in comparative example 5；
Fig. 8 is the chromatography of ions figure of the standard sample in comparative example 6.
Specific embodiment
As described above, the present invention provides a kind of analyzing detecting methods of drinking water glyphosate, which is characterized in that described
Analyzing detecting method includes the following steps:
(1) operating parameter of ion chromatograph is determined；Flow rate of mobile phase is 0.8-1.0mL/min, chromatographic column packet used
Analytical column containing AS19 and AG19 guard column.
(2) standard curve of glyphosate is made；And
(3) content of sample glyphosate is determined.
In a kind of currently preferred specific embodiment, wherein leacheate is the aqueous slkali of 20-40mmol/L；It is excellent
Choosing, the leacheate is the aqueous slkali of 30mmol/L；More preferably, the aqueous slkali is the molten of sodium hydroxide or potassium hydroxide
Liquid, the leacheate are to be produced by the automatic electrolysis generator of EG40 leacheate (or other can automatically generate leacheate equipment) is online
Raw or manual preparation potassium hydroxide (or sodium hydroxide) leacheate, wherein eluent concentration is determined by following tests method
: under the premise of guaranteeing that peak height, peak area, peak shape and the separating degree of sample peak reach perfect condition, choose most suitable dense
Degree, to ensure analysis precision, while reducing the consumption of reagent, saves consumables cost.
In a kind of currently preferred specific embodiment, wherein conductance cell temperature is 25-35 DEG C, preferably 30 DEG C；
And/or
Column temperature is 25-35 DEG C, preferably 30 DEG C；And/or
Sampling volume is 80-120 μ L, preferably 100 μ L；And/or
Inhibition electric current is 80-100mA, preferably 90mA；And/or
Analysis time is 20-40min, preferably 30min；
Wherein, sample feeding volume is determined by following tests method: guarantee the peak height of sample peak, peak area,
Under the premise of peak shape and separating degree reach perfect condition, least sampling volume is chosen, to save sample usage amount, increases detection
Number；
Flow rate of mobile phase, conductance cell temperature, analytical column column temperature are determined by following tests method: guaranteeing sample peak
Peak height, peak area, peak shape and separating degree reach perfect condition under the premise of, according to previous experience, choose most suitable stream
Speed and temperature value；
Inhibiting electric current is determined by following tests method: according to the eluent concentration determined, instrument work station is certainly
It is dynamic to calculate the inhibition current values to match.
In a kind of currently preferred specific embodiment, wherein the AS19 analytical column and AG19 guard column it is interior
Diameter is 4nm.
In a kind of currently preferred specific embodiment, wherein the standard curve of production glyphosate in step (2)
Method includes the following steps:
1) glyphosate standard reserving solution is prepared；
2) aspiration step 1) in Standard Reserving Solution obtain standard solution with water constant volume；
3) it takes the standard solution of step 2) to be diluted respectively, obtains standard solution；
4) standard solution is analyzed using ion chromatograph, draws standard curve.
In more preferably a kind of specific embodiment of the present invention, wherein in step 1), the glyphosate standard reserve
The concentration of liquid is 100-500mg/L, preferably 100mg/L, it is further preferred that the glyphosate standard reserving solution is to have card to mark
Quasi- substance has card standard sample.
In more preferably a kind of specific embodiment of the present invention, wherein in step 2), the glyphosate standard is used
The concentration of liquid is 10-50mg/L, preferably 10mg/L；It is further preferred that drawing the Standard Reserving Solution of 1.0mL step 1), use
For pure water constant volume to 10.0mL, the concentration for obtaining glyphosate standard solution is 10-100mg/L, preferably 10mg/L.
In a kind of currently preferred specific embodiment, wherein in step 3), the concentration point of the standard solution
It Wei not 0mg/L, 0.02-0.05mg/L, 0.08-0.10mg/L, 0.15-0.25mg/L, 0.30-0.50mg/L, 0.80-
1.00mg/L and 1.50-2.00mg/L, it is preferred that the concentration of the standard solution solution is 0mg/L, 0.05mg/L, 0.10mg/
L, 0.20mg/L, 0.50mg/L, 1.00mg/L and 2.00mg/L；It is further preferred that the volume of standard solution is respectively as follows:
0mL, 0.02-0.05mL, 0.08-0.10mL, 0.15-0.25mL, 0.30-0.50mL, 0.80-1.00mL and 1.50-2.00mL,
Preferably, the volume of the standard solution is 0mL, 0.05mL, 0.10mL, 0.20mL, 0.50mL, 1.00mL and 2.00mL.
In more preferably a kind of specific embodiment of the present invention, the side of the standard curve of production glyphosate in step (2)
Method includes the following steps:
1) glyphosate Standard Reserving Solution [ρ=100.0mg/L]: purchase certified reference material or standard sample configuration set 4 DEG C
Refrigerator saves.
2) glyphosate standard solution: drawing the Standard Reserving Solution of 1.0mL step 1), with pure water constant volume to 10.0mL, this
Standard solution 10.0mg/L containing glyphosate, the same day newly match.
3) 0.00,0.05,0.10,0.20,0.50, the 1.00 and 2.00mL of standard solution of step b) is taken respectively, and use is pure
Water constant volume is to 10.0mL.This series standard solution concentration is respectively 0.0,0.05,0.10,0.20,0.50,1.00 and 2.00mg/
L, the same day newly match.
4) using ion chromatograph, to the series standard solution prepared, sample introduction is analyzed respectively, right with peak height or peak area (Y)
The concentration (X) of solution draws standard curve, or calculates regression curve.
In a kind of currently preferred specific embodiment, wherein the glyphosate and other anion in water sample are with hydrogen
Potassium oxide (or sodium hydroxide) leacheate enters anion exchange separation system (being formed by protecting with analytical column).According to analysis
Column separates the affinity difference of each ion.Separated anionic current is system converting high electric at having through Anion separation
The strong acid of conductance, and leacheate is then converted to the water of low conductivity, and the conductance of various the anionic components is measured by electric conductivity detector
Rate, qualitative with retention time, peak area or peak height are quantitative.
In a kind of currently preferred specific embodiment, wherein carrier is nitrogen.
It below to the manufacturer of raw material used in the present embodiment, is described as follows, wherein the chemical substance does not have
Have indicate be conventional reagent the pure rank of chemistry.The information and experimental facilities of raw material used in embodiment are respectively such as table 1
With shown in table 2.
The information of used raw material in 1 embodiment of table
Used experimental facilities in 2 embodiment of table
The analyzing detecting method of embodiment 1-1 measurement sample glyphosate
(1) determine the operating parameter of ion chromatograph: leacheate is the potassium hydroxide solution of 30mmol/L, mobile phase stream
Speed: 1.0mL/min, sampling volume: 100 μ L, conductance cell temperature: 30.0 DEG C, column temperature: 30.0 DEG C, anion is electrolysed continuously automatically
Regenerating the inhibition electric current that micro-membrane suppressor generates is 90mA, runing time 30min；Used reagent is pure water: redistilled water
It is prepared using Milli-Q ultrapure water machine (French Millipore Corp.), resistivity > 18.0M Ω cm, is free of object ion, warp
0.2 μm of membrane filtration
(2) glyphosate standard curve is made:
1) by glyphosate Standard Reserving Solution [ρ=100.0mg/L], 4 DEG C of refrigerators is set and are saved.
2) glyphosate standard solution: 1.0mL glyphosate Standard Reserving Solution is drawn, with pure water constant volume to 10.0mL, the mark
Standard uses liquid 10.0mg/L containing glyphosate, and the same day newly matches.
3) standard solution: 0.00,0.05,0.10,0.16,0.40,0.80 and of glyphosate standard solution is taken respectively
1.60mL, with pure water constant volume to 10.0mL, this series standard solution concentration is 0.0,0.05,0.10,0.20,0.50,1.00 He
2.00mg/L, the same day newly match.
4) the series of standards solution of step 3) is distinguished into sample introduction, standard is drawn with concentration (X) of the peak area (Y) to solution
Curve, curve are as shown in Figure 1, wherein concentration be 1.00mg/L standard solution sample introduction after obtained chromatography of ions figure such as
Shown in Fig. 2.
It will be seen from figure 1 that glyphosate linear relationship in the range of 0-2.0mg/L is good (r > 0.9990).
Figure it is seen that the peak shape of obtained chromatography of ions figure is regular, separating degree is suitable (separating degree 2.32),
It is quantitative to be conducive to numerical value, and analysis time is more appropriate.
(3) content of sample glyphosate is determined
1) water sampling and store method
It is stored after sample acquisition using polypropylene containers, the sodium thiosulfate that 100mg/L is added can eliminate chlorine bring shadow
It rings.In the environment that sample should be stored in 4 DEG C, be protected from light, and measure within 2 weeks.
2) sample pretreatment: by water sample through 0.2 μm of membrane filtration, then pretreated water sample injects sampling system, point
The analysis time is 30min, peak height and peak area is recorded, according to calibration curve equation, to obtain the content of water sample glyphosate.
The analyzing detecting method of embodiment 1-2 measurement sample glyphosate
Embodiment 1-2 is identical as the operating procedure of embodiment 1-1, and difference is, flow rate of mobile phase 0.8mL/min,
Leacheate is 20mmol/L sodium hydroxide solution, and conductance cell temperature is 25 DEG C, and column temperature is 25 DEG C, and sampling volume is 80 μ L, is inhibited
Electric current is 80mA and analysis time is 20min.
The analyzing detecting method of embodiment 1-3 measurement sample glyphosate
Embodiment 1-3 is identical as the operating procedure of embodiment 1-1, and difference is, flow rate of mobile phase 0.9mL/min,
Leacheate is 40mmol/L sodium hydroxide solution, and conductance cell temperature is 35 DEG C, and column temperature is 35 DEG C, and sampling volume is 120 μ L, is inhibited
Electric current is 100mA and analysis time is 40min.
2 methodology validation of embodiment
1) detection limit and Determination Limit
Concentration when being 3:1 that detection limit is signal-to-noise ratio, calculation formula D=3N/S, N- noise in formula, S- signal response,
D- minimal detectable concentration is detected using the concentration of 0.05mg/mL, obtains detection limit 0.006mg/L, and Determination Limit is inspection
4 times of rising limit, i.e. Determination Limit are 0.024mg/L.
2) Precision Experiment
The glyphosate standard sample for taking tri- concentration of glyphosate 0.10mg/L, 0.80mg/L, 1.50mg/L is continuously done 6 times
Precision Experiment, testing result are as shown in table 3.
3 precision test data of table
From table 3 it can be seen that the standard deviation of tri- measurement of concetrations of glyphosate 0.10mg/L, 0.80mg/L, 1.00mg/L
Respectively 0.003mg/L, 0.011mg/L, 0.020mg/L, relative standard deviation 3.12%, 1.37%, 1.90%.
3) recovery of standard addition is tested
Under the chromatographic condition described in embodiment 1-1, carry out to the sample of 1-6 the measurement of glyphosate content, carries out
Recovery of standard addition experiment, the results are shown in Table 4.
4 actual sample mark-on test data of table
From table 4, it can be seen that the recovery of standard addition of three concentration of 0.250mg/L, 0.650mg/L and 1.50mg/mL point
It Wei 98.8%, 100%, 101%.
Comparative example 1
Comparative example 1 is identical as the operating procedure of embodiment 1-1, and difference is, flow rate of mobile phase 0.5mL/min, institute
The chromatography of ions figure of obtained standard sample is as shown in Figure 3.
Comparative example 2
Comparative example 2 is identical as the operating procedure of embodiment 1-1, and difference is, flow rate of mobile phase 1.2mL/min, institute
The chromatography of ions figure of obtained standard sample is as shown in Figure 4.
Comparative example 3
Comparative example 3 is identical as the operating procedure of embodiment 1-1, and difference is, sampling volume is 25 μ L, obtained mark
The chromatography of ions figure of quasi- sample is as shown in Figure 5.
4 comparative example 4 of comparative example is identical as the operating procedure of embodiment 1-1, and difference is, sampling volume is 50 μ L, institute
The chromatography of ions figure of obtained standard sample is as shown in Figure 6.
Comparative example 5
Comparative example 5 is identical as the operating procedure of embodiment 1-1, and difference is, sampling volume is 125 μ L, obtained
The chromatography of ions figure of standard sample is as shown in Figure 7.
Comparative example 6
Comparative example 6 is identical as the operating procedure of embodiment 1-1, and difference is, is protected using AS11 analytical column and AS11
Column (silent winged purchased from match), the chromatography of ions figure of obtained standard sample is as shown in Figure 8.
Embodiment 1-1, comparative example 1 and comparative example 2 are compared, difference is the difference of flow velocity, embodiment 1-1's
Flow velocity is 1.0mL/min, and the flow velocity of comparative example 1 is 0.5mL/min, and the flow velocity of comparative example is 1.2mL/min, obtained standard
The chromatography of ions figure of sample is respectively as shown in Fig. 2, Fig. 3 and Fig. 4.
By the comparison of Fig. 2,3,4 it is found that when flow velocity is 1.0mL/min, peak shape is regular, and separating degree is suitable, and (separating degree is
2.32) it is quantitative, to be conducive to numerical value, and analysis time is more appropriate；When flow velocity is 0.5mL/min, although the higher (separation of separating degree
3.04) degree is, but peak shape is irregular, leads to quantitative inaccuracy, and analysis time is too long, is unfavorable for the inspection of batch samples
It surveys；When flow velocity is 1.2mL/min, although analysis time is shorter, peak shape is excessively elongated, and forked situation occurs, separation
It spends smaller (separating degree 2.06), the masking interference being likely to result between different material peak influences quantifying for target peak.
Embodiment 1-1, comparative example 3 to comparative example 5 are compared, difference is the difference of sampling volume, comparative example 3
Sampling volume is 25 μ L, and the sampling volume of comparative example 4 is 50 μ L, and the sampling volume in comparative example 5 is 125 μ L, embodiment 1-1's
Sampling volume is 100 μ L, and the chromatography of ions figure of obtained standard sample is respectively such as Fig. 5, shown in Fig. 6, Fig. 7 and Fig. 2.
It can be seen that the glyphosate not appearance when sample volume is 25 μ L from Fig. 5, Fig. 6, Fig. 7 and Fig. 2；When sampling volume is
When 50 μ L, glyphosate appearance, but peak area is smaller, is unfavorable for quantitative integration；When sampling volume is 125 μ L, although appearance
Effect and the appearance effect of Fig. 2 are not much different, but since sample volume is larger, increases the consumption of reagent, improve cost.It will
Embodiment 1-1 and comparative example 6 compare, and difference is that embodiment 1-1 uses AS19 analytical column+AG19 guard column,
And comparative example 6 uses AS11 analytical column+AG11 guard column, the chromatography of ions figure of obtained standard sample is respectively such as Fig. 2
With shown in Fig. 8.
It can be seen that from Fig. 2 and Fig. 8 using AS11 analytical column+AG11 guard column, although analysis time is shorter, peak
Type is imperfect, has shoulder seam appearance, and bad with the separating degree of adjacent peak, and uses the peak type of AS19 analytical column+AG19 guard column
Completely, area is larger, is conducive to quantitative analysis.
In conclusion, recovery of standard addition 98.8- small using the standard deviation of analyzing detecting method of the present invention
101%, be conducive to the detection of batch samples, and present invention employs AS19 analytical column and AG19 guard column, increase into
Sample amount optimizes the temperature of column temperature and conductance cell, so that the present invention has more practicability and generalization.
The above is only the preferred embodiment that the present invention is implemented, and not does limitation in any form to the present invention, all
The modifications, equivalent substitutions and improvements etc. done within the spirit and principles in the present invention are required to be included in protection of the invention
Within the scope of.
Claims (10)
1. a kind of analyzing detecting method of drinking water glyphosate, which is characterized in that the analyzing detecting method includes following steps
It is rapid:
(1) operating parameter of ion chromatograph is determined；Flow rate of mobile phase is 0.8-1.0mL/min, and chromatographic column used includes
AS19 analytical column and AG19 guard column；
(2) standard curve of glyphosate is made；And
(3) content of sample glyphosate is determined.
2. analyzing detecting method according to claim 1, wherein leacheate is the aqueous slkali of 20-40mmol/L；It is preferred that
, the leacheate is the aqueous slkali of 30mmol/L；More preferably, the aqueous slkali is the molten of sodium hydroxide or potassium hydroxide
Liquid.
3. analyzing detecting method according to claim 1 or 2, wherein conductance cell temperature is 25-35 DEG C, preferably 30 DEG C；
And/or
Column temperature is 25-35 DEG C, preferably 30 DEG C；And/or
Sampling volume is 80-120 μ L, preferably 100 μ L；And/or
Inhibition electric current is 80-100mA, preferably 90mA；And/or
Analysis time is 20-40min, preferably 30min.
4. according to claim 1 any one of -3 analyzing detecting method, wherein the AS19 analytical column and AG19 guard column
Internal diameter is 4nm.
5. the analyzing detecting method of any one of -4 institutes according to claim 1, wherein the standard song of production glyphosate in step (2)
The method of line includes the following steps:
1) glyphosate standard reserving solution is prepared；
2) aspiration step 1) in Standard Reserving Solution obtain standard solution with water constant volume；
3) it takes the standard solution of step 2) to be diluted respectively, obtains standard solution；
4) standard solution is analyzed using ion chromatograph, draws standard curve.
6. analyzing detecting method according to claim 5, wherein in step 1), the glyphosate Standard Reserving Solution
Concentration is 100-500mg/L, preferably 100mg/L, it is further preferred that the glyphosate standard reserving solution is to have card reference substance
Matter has card standard sample.
7. analyzing detecting method according to claim 5 or 6, wherein in step 2), the glyphosate standard solution
Concentration be 10-50mg/L, preferably 10mg/L.
8. according to the described in any item analyzing detecting methods of claim 5-7, wherein in step 3), the standard solution
Concentration is respectively 0mg/L, 0.02-0.05mg/L, 0.08-0.10mg/L, 0.15-0.25mg/L, 0.30-0.50mg/L, 0.80-
1.00mg/L and 1.50-2.00mg/L, it is preferred that the concentration of the standard solution solution is 0mg/L, 0.05mg/L, 0.10mg/
L, 0.20mg/L, 0.50mg/L, 1.00mg/L and 2.00mg/L.
9. according to the described in any item analyzing detecting methods of claim 5-8, wherein in step 3), the body of standard solution
Product be respectively as follows: 0mL, 0.02-0.05mL, 0.08-0.10mL, 0.15-0.25mL, 0.30-0.50mL, 0.80-1.00mL and
1.50-2.00mL, it is preferred that the volume of the standard solution be 0mL, 0.05mL, 0.10mL, 0.20mL, 0.50mL,
1.00mL and 2.00mL.
10. -9 described in any item analyzing detecting methods according to claim 1, wherein carrier gas is nitrogen.
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