CN112129859B - Method for detecting residual quantity of pyriproxyfen in tea - Google Patents

Method for detecting residual quantity of pyriproxyfen in tea Download PDF

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CN112129859B
CN112129859B CN202011108868.5A CN202011108868A CN112129859B CN 112129859 B CN112129859 B CN 112129859B CN 202011108868 A CN202011108868 A CN 202011108868A CN 112129859 B CN112129859 B CN 112129859B
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tea
pyriproxyfen
detecting
residual quantity
blank matrix
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CN112129859A (en
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王小明
张辉
乔琳
周风达
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Anhui Huachen Testing Technology Research Institute Co ltd
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Abstract

The invention discloses a method for detecting the residual quantity of pyriproxyfen in tea, which adopts a high performance liquid chromatography-mass spectrometry combined method for detection and carries out an addition recovery test in fresh tea and dry tea, wherein: the recovery rate of the pyriproxyfen on the fresh tea is 90-111%, and the RSD is 1-4%; the recovery rate on the dried tea is 91-99%, and the RSD is 1-3%. The invention provides a convenient and reliable detection method for researching the change of the residual quantity of the tea after the pyriproxyfen is applied.

Description

Method for detecting residual quantity of pyriproxyfen in tea
Technical Field
The invention relates to the technical field of pesticide residue detection, in particular to a method for detecting the residual quantity of pyriproxyfen in tea.
Background
Pyriproxyfen is also known as pyriproxyfen, is an insect growth regulator, belongs to the third generation of pesticide, has the characteristics of low toxicity, high efficiency, long acting and the like, and is used for controlling pests of homoptera, thysanoptera, diptera, lepidoptera and the like. The detection methods of pyriproxyfen reported in domestic and foreign data documents include liquid chromatography, gas chromatography-mass spectrometry combined method and liquid chromatography-mass spectrometry combined method. However, no research report about a detection method of a tea matrix is found, the tea matrix is relatively complex, a large amount of time is consumed in sample purification by a liquid chromatography, a gas chromatography and a gas chromatography-mass spectrometry combined method, great workload is brought to detection work, and interference of impurities in tea cannot be effectively removed in a pretreatment process of the existing liquid chromatography-mass spectrometry combined method. In order to research the change of the residual quantity of the tea after the application of the pyriproxyfen, a convenient and accurate detection method suitable for a tea matrix needs to be researched.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for detecting the residual quantity of pyriproxyfen in tea, and the method can be used for simultaneously, simply, rapidly and accurately detecting the residual quantity of pyriproxyfen in a tea matrix.
The invention provides a method for detecting the residual quantity of pyriproxyfen in tea, 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 15, 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 ion source is a positive ion mode, the interface voltage is 4.5kv, the DL tube temperature is 250 ℃, the heating block temperature is 400 ℃, the interface temperature is 300 ℃, the atomization gas flow is 3L/min, the drying gas flow is 10L/min, the heating gas flow is 10L/min, and the collision gas is argon gas; the monitoring mode is a multi-reaction monitoring mode.
Preferably, the multiple reaction monitoring conditions of pyriproxyfen are: selecting an ion pair with a mass-to-charge ratio of 322.10>96.00 and 322.10>227.10 as a qualitative ion pair, and selecting an ion pair with a mass-to-charge ratio of 322.10>, 96.00 as a quantitative ion pair; wherein the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 322.10> -96.00 are respectively-30V, -30 and-23V, the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 322.10> -227.10 are respectively-30V, -14 and-17V, and the residence time is 100msec.
The symbol ">" in the above-mentioned 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 column is of the type Shim-pack GIST C18, the column specification is 2.1mm X100 mm, 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 high performance liquid chromatography collection time is less than or equal to 4min.
Preferably, the specific detection steps are: taking pyriproxyfen standard substances, preparing series of standard working solutions with different concentrations by using tea blank matrix extracting solution, sampling and drawing a standard curve to obtain a linear regression equation, sampling the tea extracting solution to be detected, and calculating the content of pyriproxyfen in tea by using the linear regression equation.
Preferably, the tea leaf blank matrix refers to a sample of tea leaves that does not contain pyriproxyfen.
Preferably, the preparation method of the tea blank matrix extracting solution is the same as that of the tea extracting solution to be detected, and the preparation method comprises the following steps: weighing 1.000g of crushed and uniformly mixed tea blank matrix or tea to be detected, uniformly mixing the tea blank matrix or the tea to be detected with 10mL of formic acid acetonitrile solution with the formic acid volume fraction of 1%, oscillating and extracting for 30min, then adding 0.5g of sodium chloride, vortex and uniformly mixing, centrifuging, transferring 1-2 mL of supernate, vortex and uniformly mixing with 50mg of N-propyl ethylenediamine, 50mg of octadecylsilane chemically bonded silica, 50mg of graphitized carbon black and 150mg of anhydrous magnesium sulfate, standing, taking the supernate, and filtering with an organic filter membrane of 0.22 mu m.
Preferably, the tea leaves are fresh tea leaves or dry tea leaves.
Fresh tea leaves refer to untreated tea leaves picked directly from tea trees, and dry tea leaves refer to tea leaves obtained by drying, dehydrating or simply processing fresh tea leaves.
To prove the effectiveness of the verification method, a test of adding pyriproxyfen into tea leaves for recovery is carried out, and the results are as follows:
when the addition concentration of the pyriproxyfen on the fresh tea is 0.05mg/kg, 1mg/kg and 15mg/kg, the average recovery rate is 90-111 percent, and the RSD is 1-4 percent; when the addition concentration of the tea leaves on the dried tea leaves is 0.05mg/kg, 1mg/kg or 15mg/kg, the average recovery rate is 91-99% and the RSD is 1-3%.
The quantitative limit of the pyriproxyfen in fresh tea and dry tea is 0.05mg/kg, the minimum detection amount is 5pg, and the quantitative limit can meet the requirement of the domestic maximum residual limit (the maximum residual limit of the pyriproxyfen in the tea is 1mg/kg in GB 2763-2019).
Test results show that the residue analysis method meets the requirements of 'test criteria of pesticide residue in crops' (NY/T788-2018), and can be used for development of pesticide residue tests.
Has the advantages that:
the invention uses LC-MS/MS (high performance liquid chromatography-mass spectrometry) analysis technology, finds out instrument data acquisition conditions which are not mutually influenced according to the properties of compounds, and simultaneously determines the quality of a substance to be detected through retention time and ion abundance ratio; the method selects proper extraction reagent (acetonitrile formate solution), extraction reagent (sodium chloride) and purification reagent (ethylenediamine-N-propyl, octadecylsilane chemically bonded silica, graphitized carbon black and anhydrous magnesium sulfate) to remove complicated pretreatment processes; the detection condition of the instrument is optimized, and the sensitivity and the resolution capability of the instrument are improved; the method can simply, quickly and accurately detect the pyriproxyfen in the matrix of the fresh tea or the dry tea.
Drawings
Figure 1 is a standard curve of pyriproxyfen in a standard working solution of fresh tea leaves of example 1.
Figure 2 is a standard curve for pyriproxyfen in a standard working solution of dry tea leaves according to example 1.
FIG. 3 is an extracted ion current chromatogram (EIC) of an air-white solvent in example 1.
FIG. 4 is an extracted ion current chromatogram (EIC) of the blank matrix extract of fresh tea leaves in example 1.
Fig. 5 is an extracted ion current chromatogram (EIC) of pyriproxyfen in the standard working solution of fresh tea leaves of example 1.
Fig. 6 is an extraction ion current chromatogram (EIC) of the fresh tea extract to be tested in example 1.
FIG. 7 is an extracted ion current chromatogram (EIC) of the blank matrix extract of dried tea leaves of example 1.
Fig. 8 is an extracted ion current chromatogram (EIC) of pyriproxyfen in a standard working solution of dry tea leaves of example 1.
FIG. 9 is an extracted ion current chromatogram (EIC) of the dried tea extract to be tested in example 1.
FIG. 10 is an extracted ion current chromatogram (EIC) of an extract of fresh tea leaf sample A in example 2.
FIG. 11 is an extracted ion current chromatogram (EIC) of an extract of fresh tea leaf sample B in example 2.
FIG. 12 is an extracted ion current chromatogram (EIC) of an extract of fresh tea leaf sample C in example 2.
FIG. 13 is an extracted ion current chromatogram (EIC) of an extract of fresh tea leaf sample D in example 2.
FIG. 14 is an extracted ion current chromatogram (EIC) of the extract of fresh tea leaf sample E in example 2.
FIG. 15 is an extracted ion current chromatogram (EIC) of an extract of fresh tea leaf sample F in example 2.
FIG. 16 is an extracted ion current chromatogram (EIC) of an extract of a dried tea leaf sample A in example 3.
FIG. 17 is an extracted ion current chromatogram (EIC) of an extract of a dried tea sample B in example 3.
FIG. 18 is an extracted ion current chromatogram (EIC) of an extract of a dried tea leaf sample C in example 3.
FIG. 19 is an extracted ion current chromatogram (EIC) of an extract of a dried tea leaf sample D in example 3.
FIG. 20 is an extracted ion current chromatogram (EIC) of an extract of a dried tea leaf sample E in example 3.
FIG. 21 is an extracted ion current chromatogram (EIC) of an extract of a dried tea leaf sample F in example 3.
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;
hundredth electronic balance (JY 5002), shunhua Hengzheng scientific instruments, inc., shanghai;
one in ten-thousandth electronic balance (AUW-220D), shimadzu corporation, japan;
an electric heating constant temperature air-blast drying box (DGH-9140A), shanghai Sanjie scientific instruments Co., ltd;
centrifuge (LD 5-2B), beijing Rebo medical devices, inc.;
water bath constant temperature oscillator (SHZ-82), yozhou guyu instruments manufacturing ltd;
ultrasonic cleaner (JK-500 DB), nikken mechanical products Co., ltd.;
VORTEX apparatus (VORTEX-2), GENIE corporation;
pipettor (100/200/1000/5000. Mu.L), eppendorf;
food processor (JR 05-300), shaoxing Supor Life appliances, inc. of Zhejiang.
The main reagents are as follows:
pyriproxyfen standard substance (purity 98.5%); acetonitrile (chromatographically pure); acetonitrile (analytical grade); formic acid (chromatographically pure); sodium chloride (analytically pure); pure water (primary water); a purge tube (containing 50mg of ethylenediamine-N-propyl group, 50mg of octadecylsilane chemically bonded silica, 50mg of graphitized carbon black, and 150mg of anhydrous magnesium sulfate).
Example 1
A method for detecting the residual quantity of pyriproxyfen in tea adopts a liquid chromatography tandem mass spectrometer LCMS-8050 of Shimadzu corporation in Japan, 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 15, 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 4min;
the mass spectrum conditions are as follows: the ion source is an electrospray ion source under atmospheric pressure, the ion source is a positive ion mode, the interface voltage is 4.5kv, the DL tube temperature is 250 ℃, the heating block temperature is 400 ℃, the interface temperature is 300 ℃, the atomizing gas flow is 3L/min, the drying gas flow is 10L/min, the heating gas flow is 10L/min, and the collision gas is argon; the monitoring mode is a multi-reaction monitoring mode (MRM);
the multiple reaction monitoring conditions for pyriproxyfen are shown in table 1.
TABLE 1 multiple reaction monitoring conditions for pyriproxyfen
Figure BDA0002727891280000061
Note: plus "indicates the quantification of the ion.
Solution preparation:
blank solvent: formic acid acetonitrile solution with formic acid volume fraction of 1%.
The fresh tea leaf sample to be tested and the blank matrix sample are picked in a tea leaf test field, and the fresh tea leaf is dried and dehydrated or simply processed to be made into dry tea leaf.
Sample preparation: mixing dry tea or fresh tea in stainless steel basin, dividing the sample by quartering method, pulverizing with pulverizer, packaging into self-sealing bag, labeling, and freezing at-18 deg.C or below.
Fresh tea blank matrix extracting solution: taking the crushed fresh tea blank matrix, recovering the crushed fresh tea blank matrix to room temperature, fully and uniformly mixing the crushed fresh tea blank matrix again, precisely weighing 1.000g of the crushed and uniformly mixed fresh tea blank matrix in a 50mL centrifugal tube, adding 10mL of formic acid acetonitrile solution with the volume fraction of 1% formic acid, uniformly mixing the mixture for 1min in a vortex manner, oscillating the mixture for 30min in an oscillator, adding 0.5g of sodium chloride, uniformly mixing the mixture for 1min in a vortex manner, and then centrifuging the mixture for 5min at the speed of 4000 r/min; precisely transferring 1.5mL of supernatant into a centrifugal tube filled with 50mg of ethylenediamine-N-propyl, 50mg of octadecylsilane chemically bonded silica, 50mg of graphitized carbon black and 150mg of anhydrous magnesium sulfate, swirling for 1min, standing for 5min, and filtering the supernatant through a 0.22-micron organic filter membrane to obtain a tea leaf blank matrix extracting solution.
Fresh tea extract to be detected: taking the crushed fresh tea leaves to be tested to return to room temperature, fully and uniformly mixing the crushed fresh tea leaves again, precisely weighing 1.001g of the crushed and uniformly mixed fresh tea leaf blank matrix into a 50mL centrifuge tube, adding 10mL of formic acid acetonitrile solution with the volume fraction of formic acid of 1%, uniformly mixing the mixture in a vortex manner for 1min, oscillating the mixture in an oscillator for 30min, adding 0.5g of sodium chloride, uniformly mixing the mixture in a vortex manner for 1min, and then centrifuging the mixture for 5min at the speed of 4000 r/min; precisely transferring 1.5mL of supernatant into a centrifugal tube filled with 50mg of ethylenediamine-N-propyl, 50mg of octadecylsilane chemically bonded silica, 50mg of graphitized carbon black and 150mg of anhydrous magnesium sulfate, swirling for 1min, standing for 5min, and filtering the supernatant with a 0.22 mu m organic filter membrane to obtain the fresh tea extract to be detected.
Extracting the blank matrix of the dry tea leaves: replacing blank matrix of fresh tea with blank matrix of dry tea, and preparing extractive solution of the blank matrix of fresh tea.
The dry tea extract to be tested: and replacing the fresh tea leaves to be detected with the dry tea leaves to be detected, and preparing the other fresh tea leaves to be detected with the extracting solution of the fresh tea leaves to be detected.
Fresh tea leaf standard working solution: respectively weighing a proper amount of pyriproxyfen standard substances (accurate to 0.00001 g), and respectively dissolving with chromatographic pure acetonitrile to prepare standard stock solutions with the concentration of 1000 mg/L; and precisely transferring a proper amount of standard stock solution into a volumetric flask, diluting with the fresh tea blank matrix extracting solution, fixing the volume, and preparing into series of standard working solutions with different concentrations.
Dry tea standard working solution: respectively weighing a proper amount of pyriproxyfen standard substances (accurate to 0.00001 g), and respectively dissolving with chromatographic pure acetonitrile to prepare standard stock solutions with the concentration of 1000 mg/L; and precisely transferring a proper amount of standard stock solution into a volumetric flask, diluting with the blank matrix extracting solution of the dry tea leaves, fixing the volume, and preparing into 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 an instrument is stabilized, and sequentially collecting a blank solvent, a fresh tea blank matrix extracting solution, a series of fresh tea standard working solutions and a fresh tea extracting solution to be detected; a blank solvent, a dry tea blank matrix extracting solution, a series of dry tea standard working solutions and a dry tea extracting solution to be detected; analyzing the collected data, drawing a standard curve to obtain a linear regression equation, and calculating the content of the pyriproxyfen in the fresh/dry tea leaves to be detected according to the linear regression equation by an external standard method.
FIG. 1 is a standard curve of pyriproxyfen in the standard working solution of fresh tea leaves in example 1, the abscissa is the concentration X of pyriproxyfen standard substance, the ordinate is the peak area y of pyriproxyfen standard substance, the linear regression equation obtained is y =29995800x +108117, R < R > 2 ＝0.9997。
FIG. 2 is a standard curve of pyriproxyfen in the standard working solution of dry tea leaves in example 1, wherein the abscissa is the concentration X of pyriproxyfen standard substance, the ordinate is the peak area y of pyriproxyfen standard substance, the linear regression equation obtained is y =31115300x +163294, R = 31100x + 2 ＝0.9998。
The concentration, peak area and linear regression equation of pyriproxyfen in the fresh/dry tea standard working solution are shown in table 2.
TABLE 2
Figure BDA0002727891280000081
The concentration C of pyriproxyfen in the fresh/dry tea extract to be detected can be calculated according to the linear regression equation Test object Then, the residue X of the pyriproxyfen in the fresh/dry tea leaves to be detected is calculated according to the following formula Test object 。
The calculation formula of the pyriproxyfen residue in the fresh/dry tea to be detected is as follows:
X test object ＝C Test object ×V 0 /m Tea leaves
In the formula:
X test object -the residual amount of the test substance in mg/kg in fresh/dry tea leaves;
C test object -the concentration of the test substance in mg/L in the fresh/dry tea extract;
V 0 -when preparing fresh/dry tea extract,volume of extraction reagent added, L;
m tea leaves Weighing the mass of the fresh/dry tea leaves to be tested, kg.
The content of pyriproxyfen in the fresh tea and the dry tea is respectively 0.059mg/kg and 0.903mg/kg.
Typical chromatograms are shown in FIGS. 3-9.
FIG. 3 is an extracted ion current chromatogram (EIC) of an air-white solvent in example 1.
FIG. 4 is an extracted ion current chromatogram (EIC) of the blank matrix extract of fresh tea leaves in example 1.
Fig. 5 is an extracted ion flow chromatogram (EIC) of pyriproxyfen in the standard working solution of fresh tea leaves of example 1, wherein the retention time of pyriproxyfen is 2.090min.
Fig. 6 is an extracted ion current chromatogram (EIC) of the fresh tea leaf extract to be tested in example 1, wherein the retention time of pyriproxyfen is 2.091min.
FIG. 7 is an extracted ion current chromatogram (EIC) of the blank matrix extract of dried tea leaves of example 1.
Fig. 8 is an extracted ion current chromatogram (EIC) of pyriproxyfen in a standard working solution of dry tea leaves of example 1, wherein the retention time of pyriproxyfen is 2.092min.
Fig. 9 is an extracted ion current chromatogram (EIC) of the dry tea extract to be tested in example 1, wherein the retention time of pyriproxyfen is 2.091min.
Example 2 fresh tea recovery test
The residual amount of pyriproxyfen in the sample was measured by adding a sample of known concentration according to the method and detection conditions of example 1, and the recovery rate was calculated.
The experimental process comprises the following steps:
taking a blank matrix of fresh tea leaves, weighing 6 parts, weighing 1.000g of each part, numbering as A, B, C, D, E and F, then respectively diluting a standard stock solution (same as example 1) of pyriproxyfen to different concentrations, adding the diluted stock solution into the blank matrix of the fresh tea leaves A, B, C, D, E and F, and uniformly mixing to ensure that the adding concentrations of pyriproxyfen in samples A and B are both 0.05mg/kg; C. the adding concentration of pyriproxyfen in the sample D is 1.0mg/kg; E. the adding concentration of pyriproxyfen in the F sample is 15.0mg/kg; then standing the sample for 2h;
the samples A, B, C, D, E and F were obtained by treating the fresh tea leaf extract to be tested in example 1.
The blank solvent, the fresh tea blank matrix extracting solution and the fresh tea standard working solution are the same as the 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 an instrument is stabilized, and sequentially collecting a reagent blank solvent, a fresh tea blank matrix extracting solution, a series of fresh tea standard working solutions, and A, B, C, D, E and F extracting solutions; analyzing the collected data, drawing a standard curve to obtain a linear regression equation, calculating the content of pyriproxyfen in the samples A, B, C, D, E and F according to the linear regression equation by an external standard method, and calculating the recovery rate of the samples.
The sample recovery rate calculation formula is as follows:
Figure BDA0002727891280000101
in the formula: x is recovery (%); c 1 The detection value of the tea 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 fresh tea leaf recovery calculations are shown in table 3.
TABLE 3 fresh tea recovery calculation results
Figure BDA0002727891280000102
Figure BDA0002727891280000111
Typical chromatograms are shown in FIGS. 10-15.
Example 3 Dry tea recovery test
The addition recovery test was performed using dry tea leaves, and the calculated recovery was measured according to the method of example 2, and the results are shown in table 4.
TABLE 4 Dry tea recovery calculation results
Figure BDA0002727891280000112
Typical chromatograms are shown in FIGS. 16-21.
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 as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.

Claims (7)

1. A method for detecting the residual quantity of pyriproxyfen in tea 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 15, 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 ion source is a positive ion mode, the interface voltage is 4.5kv, the DL tube temperature is 250 ℃, the heating block temperature is 400 ℃, the interface temperature is 300 ℃, the atomizing gas flow is 3L/min, the drying gas flow is 10L/min, the heating gas flow is 10L/min, and the collision gas is argon; the monitoring mode is a multi-reaction monitoring mode;
the type of the column was Shim-pack GIST C18, the specification of the column was 2.1 mm. Times.100 mm, and the particle diameter was 2.0. Mu.m
The specific detection steps are as follows: taking pyriproxyfen standard substances, preparing series of standard working solutions with different concentrations by using tea blank matrix extracting solution, sampling and drawing a standard curve to obtain a linear regression equation, sampling the tea extracting solution to be detected, and calculating the content of pyriproxyfen in tea by using the linear regression equation;
the preparation method of the tea blank matrix extracting solution is the same as that of the tea extracting solution to be detected, and the method comprises the following steps: weighing 1.000g of crushed and uniformly mixed tea blank matrix or tea to be detected, uniformly mixing the ground and uniformly mixed tea blank matrix or the tea to be detected with 10mL of formic acid acetonitrile solution with the formic acid volume fraction of 1%, oscillating and extracting for 30min, adding 0.5g of sodium chloride, uniformly mixing in a vortex manner, centrifuging, transferring 1-2mL of supernatant, uniformly mixing with 50mg of N-propylethylenediamine, 50mg of octadecylsilane chemically bonded silica, 50mg of graphitized carbon black and 150mg of anhydrous magnesium sulfate in a vortex manner, standing, taking the supernatant, and passing through an organic filter membrane of 0.22 mu m.
2. The method for detecting the residual amount of pyriproxyfen in tea according to claim 1, wherein the multi-reaction monitoring conditions of pyriproxyfen are as follows: selecting ion pairs with mass-to-charge ratios of 322.10>96.00 and 322.10 >; wherein the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 322.10> -96.00 are respectively-30V, -30 and-23V, the deviation voltage of Q1pre, the deviation voltage of collision voltage CE and the deviation voltage of Q3pre corresponding to the ion pair 322.10> -227.10 are respectively-30V, -14 and-17V, and the residence time is 100msec.
3. The method for detecting the residual quantity of pyriproxyfen in tea as claimed in claim 1, wherein the column temperature is 38 ℃.
4. The method for detecting the residual quantity of pyriproxyfen in tea according to claim 1, wherein the sample volume is 1 μ L.
5. The method for detecting the residual quantity of pyriproxyfen in tea leaves according to claim 1, wherein the collection time of high performance liquid chromatography is less than or equal to 4min.
6. The method for detecting the residual quantity of pyriproxyfen in tea as claimed in claim 1, wherein the tea blank matrix is a tea sample without pyriproxyfen.
7. The method for detecting the residual amount of pyriproxyfen in tea as claimed in claim 1, wherein the tea is fresh tea or dry tea.
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