CN111965275B - Method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane - Google Patents
Method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane Download PDFInfo
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Abstract
The invention discloses a method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane, which adopts a high performance liquid chromatography-mass spectrometry combined method to detect, wherein the recovery rate of mesotrione in a sugarcane matrix is 92.9-103.0%, and the RSD is 1.1-1.4%; the recovery rate of ametryn is 101.0% -103.0%, and the RSD is 0.6% -0.7%; the recovery rate of the halosulfuron-methyl is 105.0-114.0%, and the RSD is 0.7-2.0%. Provides a reliable detection method for researching the change condition of the residual quantity of the sugarcane after being applied with the 3 medicines, and simultaneously fills the blank that the prior method can not simultaneously detect mesotrione, ametryn and halosulfuron-methyl in the sugarcane matrix.
Description
Technical Field
The invention relates to the technical field of pesticide residue detection, in particular to a method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane.
Background
Mesotrione is a pre-emergence selective herbicide and a post-emergence selective herbicide capable of inhibiting hydroxyphenylpyruvate dioxygenase, ametryn is a triazene selective systemic conduction type herbicide, halosulfuron-methyl is a sulfonylurea herbicide, and the three herbicides are compounded for use, so that the mesotrione can effectively control various field broad-leaved weeds and some gramineous weeds, and is widely applied to control various field weeds.
At present, the maximum residual limit values established for the three herbicides at home and abroad are small, and instruments with higher sensitivity are required to participate in daily detection. The detection methods for the three herbicides are reported, and mainly comprise a liquid chromatography and a liquid chromatography-mass spectrometry combined method. The liquid chromatography has high quantitative limit, and cannot meet the requirement of the maximum limit value established at home and abroad; the liquid chromatography-mass spectrometry combined method has the disadvantages of complex and fussy sample pretreatment process and long detection time consumption. Moreover, no method for simultaneously detecting the residual amounts of the three herbicides is reported, and research needs to be carried out to find a reliable method for detecting the three herbicides by aiming at the sugarcane substrate.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane.
The invention provides a method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane, which adopts a high performance liquid chromatography-mass spectrometry combined method for detection, wherein the conditions of the high performance liquid chromatography are as follows: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, the mobile phase A is a formic acid aqueous solution with the volume fraction of 0.1%, the mobile phase B is acetonitrile, the elution mode is isocratic elution, the volume ratio of the mobile phase A to the mobile phase B is 50, and the flow rate is 0.3mL/min;
the mass spectrum conditions are as follows: the ion source is an electrospray ion source under atmospheric pressure, the temperature of a DL tube is 250 ℃, the temperature of a heating block is 400 ℃, the temperature of an interface is 300 ℃, the flow of atomized gas is 3L/min, the flow of dried gas is 10L/min, the flow of heated gas is 10L/min, and collision gas is argon; the monitoring mode is a multi-reaction monitoring mode.
Preferably, the multiple reaction monitoring conditions for mesotrione are: the ion source is in a negative ion mode, the interface voltage is-3.0 kV, ion pairs with the mass-to-charge ratio of 338.00> -212.00 and 338.00> -291.00 are selected as qualitative ion pairs, and ion pairs with the mass-to-charge ratio of 338.00> -291.00 are selected as quantitative ion pairs; wherein the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and Q3pre corresponding to the ion pair 338.00> -212.00 are respectively 22V, 34V and 24V, the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and Q3pre corresponding to the ion pair 338.00> -291.00 are respectively 16V, 11V and 21V, and the residence time is 45msec.
The symbol ">" in the above-described ion pair is a symbol commonly used by those skilled in the art to represent the ion pair.
The Q1pre deviation voltage, the collision voltage CE, and the Q3pre deviation voltage are specific expressions of the liquid chromatography-mass spectrometer of shimadzu corporation, japan.
Preferably, the multiple reaction monitoring conditions of ametryn are as follows: the ion source is in a positive ion mode, the interface voltage is 4.0kV, ion pairs with mass-to-charge ratios of 228.20>68.20 and 228.20>186.20 are selected as qualitative ion pairs, and ion pairs with mass-to-charge ratios of 228.20>186.20 are selected as quantitative ion pairs; wherein the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 228.20> -68.20 are respectively-15V, -20 and-15V, the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 228.20> -186.20 are respectively-15V, -10 and-15V, and the residence time is 45msec.
Preferably, the multi-reaction monitoring conditions of halosulfuron-methyl are: the ion source is in a negative ion mode, the interface voltage is-3.0 kV, an ion pair with the mass-to-charge ratio of 432.65>153.90 and 432.65>251.90 is selected as a qualitative ion pair, and an ion pair with the mass-to-charge ratio of 432.65> -251.90 is selected as a quantitative ion pair; wherein the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and Q3pre corresponding to the ion pair 432.65>153.90 are respectively 12V, 30V and 27V, the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and Q3pre corresponding to the ion pair 432.65> -251.90 are respectively 12V, 19V and 16V, and the residence time is 45msec.
Preferably, the column is of the type Shim-pack GIST C18, the column specification is 2.1X 100mm, and the particle size is 2.0. Mu.m.
Preferably, the column temperature is 38 ℃.
Preferably, the sample size is 1 μ L.
Preferably, the collection time of the high performance liquid chromatography is less than or equal to 5min.
Preferably, the specific detection steps are: taking a mesotrione standard substance, a ametryn standard substance and a halosulfuron-methyl standard substance, preparing a series of standard working solutions with different concentrations by using a sugarcane blank matrix extracting solution, carrying out sample injection and drawing a standard curve to obtain a linear regression equation, taking a sugarcane extracting solution to be detected for sample injection, and calculating the contents of mesotrione, ametryn and halosulfuron-methyl in sugarcane by using the linear regression equation.
Preferably, the sugar cane blank matrix refers to a sample of sugar cane that is free of mesotrione, ametryn, and halosulfuron-methyl.
Preferably, the preparation method of the sugarcane blank matrix extracting solution is the same as that of the sugarcane extracting solution to be detected, and the preparation method comprises the following steps: weighing 2.000g of crushed and uniformly mixed sugarcane blank matrix or sugarcane to be detected, uniformly mixing the crushed and uniformly mixed sugarcane blank matrix or sugarcane to be detected with 10mL of formic acid acetonitrile solution with the formic acid volume fraction of 1%, oscillating and extracting for 10min, adding 1-2 g of sodium chloride, uniformly mixing in a vortex manner, centrifuging, transferring 1-2 mL of supernatant, uniformly mixing with 50mg of N-propyl ethylenediamine and 125mg of anhydrous magnesium sulfate in a vortex manner, standing, taking the supernatant, and filtering with a 0.22 mu m organic filter membrane.
To demonstrate the effectiveness of the validation method, a mesotrione, ametryn and halosulfuron-methyl addition recovery test in sugarcane was performed for this purpose, with the following results:
when the addition concentration of the mesotrione on the sugarcane is 0.02-1.0 mg/kg, the recovery rate is 92.9% -103%, and the Relative Standard Deviation (RSD) is 1.1% -1.4%; when the adding concentration of ametryn on sugarcane is 0.01-1.0 mg/kg, the recovery rate is 101% -103%, and the Relative Standard Deviation (RSD) is 0.6% -0.7%; when the adding concentration of the halosulfuron-methyl on the sugarcane is 0.01-1.0 mg/kg, the recovery rate is 105% -114%, and the Relative Standard Deviation (RSD) is 0.7% -2.0%; the recovery rate and the relative standard deviation meet the requirements of NY/T788-2018.
The minimum detection amount of mesotrione, ametryn and halosulfuron-methyl in the sugarcane is 1pg, and the limit of quantitation is 0.02mg/kg, 0.01mg/kg and 0.01mg/kg respectively; the quantitative limit can meet the requirement of the maximum residual limit at home and abroad (GB 2763-2019, the maximum residual limit of mesotrione in sugarcane is 0.05mg/kg, and the ametryn is 0.05mg/kg; but the maximum residual limit of halosulfuron-methyl in sugarcane is not established at home, so the limit value established by reference EPA is 0.01 mg/kg).
Has the advantages that:
according to the invention, an LC-MS/MS (high performance liquid chromatography-mass spectrometry) analysis technology is used, instrument data acquisition conditions which are not affected by each other are found out according to the properties of compounds, data are acquired by using a positive ion mode and a negative ion mode, and mesotrione, ametryn and halosulfuron-methyl are detected at the same time; simultaneously determining the nature of the substance to be detected through retention time and ion abundance ratio; through multiple test comparisons, proper extraction reagents (formic acid acetonitrile solution with 1% formic acid volume fraction), extraction reagents (sodium chloride) and purification reagents (ethylenediamine-N-propyl and anhydrous magnesium sulfate) are selected, and the pretreatment time of the sugarcane to be detected is shortened; the acquisition conditions of the instrument are changed, and the data acquisition time of the instrument is shortened; the method solves the problems of over-high quantification limit in a chromatographic analysis method, complex and tedious detection process and over-long detection time in a mass spectrometry analysis method, and can simultaneously, simply, quickly and accurately detect the mesotrione, the ametryn and the halosulfuron-methyl in the sugarcane matrix.
Drawings
Figure 1 is a standard curve for mesotrione in a standard working solution as in example 1.
FIG. 2 is a standard curve of ametryn in a standard working solution of example 1.
FIG. 3 is a calibration curve of halosulfuron-methyl in a standard working solution of example 1.
FIG. 4 is an ion flow chromatogram of the extracts of mesotrione, ametryn and halosulfuron-methyl in the standard working solution in example 1.
FIG. 5 is an extracted ion current chromatogram of the white solvent in example 1.
FIG. 6 is an extracted ion current chromatogram of a sugar cane blank matrix extract in example 1.
FIG. 7 is an extracted ion current chromatogram of the sugarcane extract to be tested in example 1.
FIG. 8 is an extracted ion current chromatogram of an extract liquid of sample A in example 2.
FIG. 9 is an extracted ion current chromatogram of an extract solution of sample B in example 2.
FIG. 10 is an extracted ion current chromatogram of an extract liquid of sample C in example 2.
FIG. 11 is an extracted ion current chromatogram of an extract liquid of sample D in example 2.
FIG. 12 is an extracted ion current chromatogram of an extract liquid of sample E in example 2.
FIG. 13 is an extracted ion current chromatogram of an extract solution of sample F in example 2.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
The main apparatus comprises:
liquid chromatography-mass spectrometer (LCMS-8050), shimadzu corporation, japan;
one-tenth-of-ten-thousandth electronic balance (AUW-220D), shimadzu corporation, japan;
vortex mixer (XH-D), shanghai Hano instruments, inc.;
water bath constant temperature oscillator (GY 2016-SW), manufactured by yoyo instruments ltd, japan;
centrifuge (TDZ 5-WS), hunan instruments laboratory Instrument development Co., ltd.
The main reagents are as follows:
mesotrione standard (98.5% pure); ametryn standard substance (purity 97.9%); halosulfuron-methyl standard substance (purity 98.0%); acetone (chromatographically pure); acetonitrile (chromatographically pure); formic acid (chromatographically pure); sodium chloride (analytical grade); pure water (primary water); n-propylethylenediamine (40-60 μm); anhydrous magnesium sulfate (analytical grade).
Example 1
A method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane adopts a liquid chromatography tandem mass spectrometer LCMS-8050 for detection by Shimadzu corporation, wherein the conditions of high performance liquid chromatography are as follows: the chromatographic column is a Shim-pack GIST C18 chromatographic column (2.1X 100mm,2.0 μm), the mobile phase A is formic acid aqueous solution with the volume fraction of 0.1 percent, the mobile phase B is acetonitrile, the elution mode is isocratic elution, the volume ratio of the mobile phase A to the mobile phase B is 50, and the flow rate is 0.3mL/min; the column temperature is 38 ℃, the sample injection amount is 1 mu L, and the collection time of the high performance liquid chromatography is less than or equal to 5min;
the mass spectrum conditions are as follows: the ion source is an electrospray ion source under atmospheric pressure, the temperature of a DL tube is 250 ℃, the temperature of a heating block is 400 ℃, the temperature of an interface is 300 ℃, the flow of atomized gas is 3L/min, the flow of dried gas is 10L/min, the flow of heated gas is 10L/min, and collision gas is argon; the monitoring mode is a multi-reaction monitoring mode (MRM);
the ion sources of mesotrione and halosulfuron-methyl are in a negative ion mode, and the corresponding interface voltage is-3.0 kV; the ion source of the ametryn is in a positive ion mode, and the corresponding interface voltage is 4.0kV;
the multiple reaction monitoring conditions for mesotrione, ametryn and halosulfuron-methyl are shown in table 1.
TABLE 1 multiple reaction monitoring conditions for mesotrione, ametryn and halosulfuron-methyl
Note: plus ". Sup." indicates the quantitative ion.
Solution preparation:
blank solvent: formic acid acetonitrile solution with formic acid volume fraction of 1%.
The pretreatment processes of the blank sugarcane substrate and the sugarcane to be detected are the same.
Sample preparation: taking a blank sugarcane substrate or a sugarcane sample to be detected, removing leaves, cutting the blank sugarcane substrate or the sugarcane sample into small sections with the length of less than 1cm by using a stainless steel cutter, uniformly mixing the small sections in a stainless steel basin, dividing the small sections by a quartering method, uniformly crushing the divided sample by using a crusher, sealing and storing the crushed sample, and making a mark for later use.
Extracting a sugarcane blank matrix: precisely weighing 2.001g of crushed and uniformly mixed sugarcane blank matrix into a 50mL centrifuge tube, adding 10mL of formic acid acetonitrile solution with the volume fraction of 1% formic acid, performing vortex mixing, performing oscillation extraction for 10min in an oscillator with the rotation speed of 350r/min, then adding 2g of sodium chloride, performing vortex mixing for 1min, and placing in a centrifuge for 4200r/min for centrifugation for 3min; precisely transferring 1.5mL of supernatant into a centrifugal tube filled with 50mg of N-propylethylenediamine and 125mg of anhydrous magnesium sulfate, mixing uniformly in a vortex manner, standing for 3min, taking supernatant, and filtering with a 0.22-micron organic filter membrane to obtain sugarcane blank matrix extracting solution.
The sugarcane extracting solution to be detected is as follows: precisely weighing 2.001g of crushed and uniformly mixed sugarcane to be detected in a 50mL centrifuge tube, adding 10mL of formic acid acetonitrile solution with 1% formic acid volume fraction, performing vortex mixing, performing oscillation extraction for 10min in an oscillator with the rotation speed of 350r/min, then adding 2g of sodium chloride, performing vortex mixing for 1min, and placing in a centrifuge for 4200r/min for centrifugation for 3min; precisely transferring 1.5mL of supernatant into a centrifugal tube filled with 50mg of N-propylethylenediamine and 125mg of anhydrous magnesium sulfate, uniformly mixing by vortex, standing for 3min, taking supernatant, and filtering with a 0.22-micron organic filter membrane to obtain the sugarcane extracting solution to be detected.
Standard working solution: respectively weighing (to the accuracy of 0.00001 g) a proper amount of mesotrione standard substance, ametryn standard substance and halosulfuron-methyl standard substance, respectively dissolving with chromatographic pure acetone, and sequentially preparing standard stock solutions with the concentrations of 1000 mg/L; then precisely transferring a proper amount of 3 standard stock solutions into the same volumetric flask, diluting with the sugarcane blank matrix extracting solution and fixing the volume to prepare a series of standard working solutions with different concentrations.
The operation method comprises the following steps: setting instrument parameters according to the chromatographic and mass spectrum conditions, editing a batch processing table after the instrument is stabilized, and sequentially collecting a reagent blank solvent, a sugarcane blank matrix extracting solution, a series of standard working solutions and a sugarcane extracting solution to be detected; and analyzing the acquired data, drawing a standard curve to obtain a linear regression equation, and calculating the contents of mesotrione, ametryn and halosulfuron-methyl in the sugarcane to be detected according to the linear regression equation by an external standard method.
FIG. 1 is a standard curve of mesotrione in the standard working solution of example 1, with the concentration X of mesotrione standard on the abscissa and the peak area f (X) of mesotrione standard on the ordinate, and the linear regression equation obtained is f (X) =4982480X-5739.9 2 =0.9998992; the table on the right in figure 1 is the corresponding peak areas for mesotrione at different concentrations (mg/L) in a standard working solution.
FIG. 2 is a standard curve of ametryn in the standard working solution of example 1, with the abscissa being the concentration X of ametryn standard substance and the ordinate being the area Y of peak of ametryn standard substance, and the linear regression equation obtained is f (X) =26759300X-27162.2 2 =0.9999231; the table on the right side of fig. 2 shows the peak areas corresponding to different concentrations (mg/L) of ametryn in the standard working solution.
FIG. 3 is a standard curve of halosulfuron-methyl in the standard working solution of example 1, with the abscissa being the halosulfuron-methyl standardThe concentration X of the matter is shown in the vertical coordinate as the peak area Y of the halosulfuron-methyl standard substance, the obtained linear regression equation is f (X) =8898380X-12635.2 2 =0.9998539; the table on the right side of fig. 3 is the peak areas corresponding to different concentrations (mg/L) of halosulfuron-methyl in the standard working solution.
According to the linear regression equation, the concentration C of mesotrione, ametryn and halosulfuron-methyl in the sugarcane extracting solution to be detected can be calculated Test object Then, the residual quantity X of mesotrione, ametryn and halosulfuron-methyl in the sugarcane to be detected is calculated according to the following formula Test object 。
The calculation formula of the residual quantity of mesotrione, ametryn and halosulfuron-methyl in the sugarcane to be detected is as follows:
X test object ＝C Test object ×V 0 /m Sugarcane
In the formula:
X test object -the residual amount of the test substance in mg/kg in sugarcane;
C test object -the concentration of the analyte in the sugarcane extract in mg/L;
V 0 -the volume of extraction reagent added, L, when preparing the sugarcane extract;
m sugarcane -weighing the mass, kg, of the sugarcane to be tested.
The measured contents of mesotrione, ametryn and halosulfuron-methyl in the sugarcane are 0.050mg/kg, 0.049mg/kg and 0.010mg/kg respectively.
Typical chromatograms are shown in FIGS. 4-7; FIG. 4 is an extracted ion current chromatogram (EIC) of mesotrione, ametryn and halosulfuron-methyl in the standard working solution of example 1, wherein the retention time of mesotrione is 1.372min, the retention time of ametryn is 1.654min and the retention time of halosulfuron-methyl is 2.607min.
FIG. 5 is an extracted ion current chromatogram (EIC) of an air-white solvent in example 1.
FIG. 6 is an extracted ion current chromatogram (EIC) of the sugar cane blank matrix extract in example 1.
Fig. 7 is an extraction ion current chromatogram (EIC) of a sugarcane extracting solution to be tested in example 1, wherein the retention time of mesotrione is 1.299min, the retention time of ametryn is 1.505min, and the retention time of halosulfuron-methyl is 2.441min.
Example 2 recovery test
The residual amounts of mesotrione, ametryn and halosulfuron-methyl in the samples were detected by adding samples of known concentrations according to the method and detection conditions of example 1, and the recovery rates were calculated.
The experimental process comprises the following steps:
weighing 6 parts of blank sugarcane substrate, weighing 2.000g of blank sugarcane substrate, wherein the number of the blank sugarcane substrate is A, B, C, D, E, F, respectively diluting standard stock solutions of mesotrione, ametryn and halosulfuron-methyl (same as in example 1) to different concentrations, adding the diluted stock solutions into A, B, C, D, E, F blank sugarcane substrate, and uniformly mixing the stock solutions to ensure that the adding concentrations of mesotrione, ametryn and halosulfuron-methyl in a A, B sample are 0.02mg/kg, 0.01mg/kg and 0.01mg/kg in sequence; C. d, adding the mesotrione, the ametryn and the halosulfuron-methyl in the sample D to the concentration of 0.05mg/kg; E. the adding concentrations of mesotrione, ametryn and halosulfuron-methyl in the sample F are all 1.0mg/kg; then standing the sample for 2h;
the sugarcane extract to be tested in example 1 was treated to obtain the extract of A, B, C, D, E, F samples, respectively.
The blank solvent, the sugarcane blank matrix extracting solution and the standard working solution are the same as in example 1.
The operation method comprises the following steps: setting instrument parameters according to the chromatographic and mass spectrum conditions, editing a batch processing table after the instrument is stabilized, and sequentially collecting a reagent blank solvent, a sugarcane blank matrix extracting solution, a series of standard working solutions and a A, B, C, D, E, F extracting solution; analyzing the collected data, drawing a standard curve to obtain a linear regression equation, calculating the contents of mesotrione, ametryn and halosulfuron-methyl in the A, B, C, D, E, F sample according to the linear regression equation by an external standard method, and calculating the recovery rate of the sample.
The sample recovery rate calculation formula is as follows:
in the formula: x is recovery (%); c 1 The detection value of the sugarcane blank matrix sample after pesticide is added is mg/kg; c 0 The concentration value of the actually added pesticide in the blank sample is mg/kg.
The results of the recovery calculation are shown in Table 2.
TABLE 2 results of recovery calculation
Typical chromatograms are shown in FIGS. 8-13.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane is characterized by adopting a high performance liquid chromatography-mass spectrometry combined method for detection, wherein the conditions of the high performance liquid chromatography are as follows: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, the mobile phase A is a formic acid aqueous solution with the volume fraction of 0.1%, the mobile phase B is acetonitrile, the elution mode is isocratic elution, the volume ratio of the mobile phase A to the mobile phase B is 50, and the flow rate is 0.3mL/min; the collection time of the high performance liquid chromatography is less than or equal to 5min; the type of the chromatographic column is Shim-pack GIST C18, the specification of the chromatographic column is 2.1 multiplied by 100mm, and the particle size is 2.0 mu m;
the mass spectrum conditions are as follows: the ion source is an electrospray ion source under atmospheric pressure, the temperature of a DL tube is 250 ℃, the temperature of a heating block is 400 ℃, the temperature of an interface is 300 ℃, the flow of atomized gas is 3L/min, the flow of dried gas is 10L/min, the flow of heated gas is 10L/min, and collision gas is argon; the monitoring mode is a multi-reaction monitoring mode;
the preparation method of the sugarcane blank matrix extracting solution is the same as that of the sugarcane extracting solution to be detected, and the preparation method comprises the following steps: weighing 2.000g of crushed and uniformly mixed sugarcane blank matrix or sugarcane to be detected, uniformly mixing the crushed and uniformly mixed sugarcane blank matrix or sugarcane to be detected with 10mL of formic acid acetonitrile solution with the formic acid volume fraction of 1%, oscillating and extracting for 10min, adding 1-2g of sodium chloride, uniformly mixing in a vortex manner, centrifuging, transferring 1-2mL of supernatant, uniformly mixing with 50mg of N-propylethylenediamine and 125mg of anhydrous magnesium sulfate in a vortex manner, standing, taking the supernatant, and filtering with a 0.22 mu m organic filter membrane.
2. The method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane according to claim 1, wherein the multiple reaction monitoring conditions for mesotrione are as follows: the ion source is in a negative ion mode, the interface voltage is-3.0 kV, ion pairs with the mass-to-charge ratio of 338.00> -212.00 and 338.00> -291.00 are selected as qualitative ion pairs, and ion pairs with the mass-to-charge ratio of 338.00> -291.00 are selected as quantitative ion pairs; wherein the deviation voltage of Q1pre, the collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 338.00> -212.00 are 22V, 34 and 24V respectively, the deviation voltage of Q1pre, the collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 338.00> -291.00 are 16V, 11 and 21V respectively, and the residence time is 45msec.
3. The method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane according to claim 1 or 2, wherein the multiple reaction monitoring conditions for ametryn are as follows: the ion source is in a positive ion mode, the interface voltage is 4.0kV, ion pairs with mass-to-charge ratios of 228.20>68.20 and 228.20>186.20 are selected as qualitative ion pairs, and ion pairs with mass-to-charge ratios of 228.20>186.20 are selected as quantitative ion pairs; wherein the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 228.20> -68.20 are respectively-15V, -20 and-15V, the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 228.20> -186.20 are respectively-15V, -10 and-15V, and the residence time is 45msec.
4. The method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane according to claim 1, wherein the multiple reaction monitoring conditions of halosulfuron-methyl are as follows: the ion source is in a negative ion mode, the interface voltage is-3.0 kV, ion pairs with mass-to-charge ratios of 432.65>153.90 and 432.65>251.90 are selected as qualitative ion pairs, and ion pairs with mass-to-charge ratios of 432.65>251.90 are selected as quantitative ion pairs; wherein the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 432.65> < 153.90 are respectively 12V, 30 and 27V, the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 432.65> < 251.90 are respectively 12V, 19 and 16V, and the residence time is 45msec.
5. The method for detecting mesotrione, ametryn and halosulfuron-methyl in sugar cane as claimed in claim 1, wherein the column temperature is 38 ℃.
6. The method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane according to claim 1, wherein the sample size is 1 μ L.
7. The method for detecting mesotrione, ametryn and halosulfuron-methyl in sugarcane according to claim 1, characterized by comprising the following specific detection steps: taking a mesotrione standard substance, a ametryn standard substance and a halosulfuron-methyl standard substance, preparing a series of standard working solutions with different concentrations by using a sugarcane blank matrix extracting solution, carrying out sample injection and drawing a standard curve to obtain a linear regression equation, taking a sugarcane extracting solution to be detected for sample injection, and calculating the contents of mesotrione, ametryn and halosulfuron-methyl in sugarcane by using the linear regression equation.
8. The method for detecting mesotrione, ametryn and halosulfuron-methyl in sugar cane as claimed in claim 7, wherein the sugar cane blank matrix is a sample of sugar cane that is free of mesotrione, ametryn and halosulfuron-methyl.
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