CN107831228B - Method and kit for determining citronellal in sample and application of kit - Google Patents
Method and kit for determining citronellal in sample and application of kit Download PDFInfo
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Abstract
The invention belongs to the field of detection and analysis, and particularly relates to a method for determining citronellal in a sample, which comprises the following steps: (1) dipping a sample by adopting a proper solvent, and carrying out solid-liquid separation to obtain an extracting solution; (2) detecting the extracting solution obtained in the step (1) by adopting liquid chromatography-tandem mass spectrometry to obtain a detection result; (3) qualitatively analyzing and/or quantitatively calculating citronellal in the sample according to the detection result obtained in the step (2); in the step (2), in the detection conditions of the liquid chromatography, the mobile phase consists of a mobile phase A and a mobile phase B, wherein the mobile phase A is acetonitrile, the mobile phase B is an ammonium acetate solution containing acetic acid, and the molar concentration of ammonium acetate in the mobile phase B is 1-10 mmoL/L. On the basis, the invention also provides a kit. The determination method of the invention can rapidly and accurately determine the content of citronellal in the essence and spice sample, and has high recovery rate and good reproducibility.
Description
Technical Field
The invention belongs to the field of detection and analysis, and particularly relates to a method for determining citronellal in a sample, and also relates to a kit and application thereof.
Background
Citronellal (Citronellal), also known as androstenal and 3, 7-dimethyl-6-octenal, is present in citronella oil and eucalyptus oil from eucalyptus leaves and is used for formulating flavorants (e.g., citrus and cherry flavors), soap flavors and synthetic menthol. Citronellal is widely applied to the fields of medicine, tobacco, food and the like, plays an important role in the fragrance of tobacco and is a common component of essence and flavor for tobacco.
At present, a gas chromatography-mass spectrometry (GC-MS) is mainly used for detecting citronellal, but because the components of a flavor and fragrance sample are complex, a more complicated pretreatment process (such as derivatization) is needed for detection by adopting the GC-MS, and a longer analysis time is needed for separating a target object from an interfering object baseline by the GC-MS. Based on the situation, a simple and rapid detection method for analyzing citronellal in flavors and fragrances is urgently needed.
Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is an analytical detection method that has been developed in recent years. So far, no technology for detecting citronellal in flavors and fragrances by LC-MS/MS has been found.
Disclosure of Invention
The invention provides a method for measuring citronellal in a sample, which can quickly and accurately measure the content of citronellal in an essence and spice sample, and has the advantages of good reproducibility, high recovery rate and simple and convenient operation. On the basis, the invention also provides a kit and application thereof in determination of citronellal in a sample.
The first aspect of the invention relates to a method for determining citronellal in a sample, which comprises the following steps:
(1) dipping a sample by adopting a proper solvent, and carrying out solid-liquid separation to obtain an extracting solution;
(2) detecting the extracting solution obtained in the step (1) by adopting liquid chromatography-tandem mass spectrometry to obtain a detection result;
(3) qualitatively analyzing and/or quantitatively calculating citronellal in the sample according to the detection result obtained in the step (2);
in the step (2), in the detection conditions of the liquid chromatography, the mobile phase consists of a mobile phase A and a mobile phase B, wherein the mobile phase A is acetonitrile, the mobile phase B is an ammonium acetate solution containing acetic acid, and the molar concentration of ammonium acetate in the mobile phase B is 1-10 mmoL/L.
In certain embodiments of the first aspect of the present invention, the liquid obtained by solid-liquid separation in step (1) is the extract obtained in step (1).
In certain embodiments of the first aspect of the present invention, in step (2), the detection conditions of the liquid chromatography include a molar concentration of ammonium acetate in mobile phase B of 2-8mmoL/L, such as 3, 4, 5, 6, 7, or 9 mmoL/L.
In certain embodiments of the first aspect of the present invention, in step (2), the detection conditions of the liquid chromatography include a content of acetic acid in mobile phase B of 0.05% (v/v) to 0.5% (v/v), preferably 0.08% (v/v) to 0.4% (v/v), for example 0.06% (v/v), 0.1% (v/v), 0.2% (v/v), 0.3% (v/v), 0.45% (v/v).
In certain embodiments of the first aspect of the present invention, in step (2), the detection conditions of liquid chromatography are as follows, and the elution procedure is as shown in table 1 below:
TABLE 1
In certain embodiments of the first aspect of the present invention, in step (2), the qualitative ion pair of citronellal in the tandem mass spectrometry detection conditions is 155.0>81.1 and/or 155.0> 137.2.
In certain embodiments of the first aspect of the present invention, in step (2), the quantitative ion pair of citronellal in the tandem mass spectrometry detection conditions is 155.0> 81.1.
In certain embodiments of the first aspect of the present invention, wherein step (2) further comprises one or more of the following a) to m):
a) the liquid chromatography is high performance liquid chromatography;
b) in the detection conditions of the liquid chromatogram, a chromatographic column is a C18 chromatographic column, preferably a Philomena C18 chromatographic column, and the specification is 50mm × 2.1.1 mm i.d., and the particle size is 2.6 mu m;
c) in the detection conditions of the liquid chromatography, the temperature of a chromatographic column is 20-40 ℃, preferably 28-32 ℃, such as 22 ℃, 23 ℃, 25 ℃, 27 ℃, 29 ℃, 30 ℃ or 31 ℃;
d) in the detection conditions of the liquid chromatography, the flow rate is 0.1-1mL/min, preferably 0.1-0.5mL/min, such as 0.2mL/min, 0.3mL/min, 0.4mL/min, 0.6mL/min, 0.8mL/min or 0.9 mL/min;
e) the tandem mass spectrum is a triple quadrupole mass spectrum;
f) in the detection condition of the tandem mass spectrum, an ion source is an electrospray ionization source;
g) in the detection condition of the tandem mass spectrum, the scanning mode is positive ion scanning;
h) in the detection condition of the tandem mass spectrum, the detection mode is multi-reaction monitoring;
i) in the detection conditions of the tandem mass spectrum, the electrospray voltage is 3500-4500V, preferably 4000V;
j) in the detection condition of the tandem mass spectrum, the temperature of an ion source is 300-500 ℃, and preferably 400 ℃;
k) the detection conditions of the tandem mass spectrometry are that the auxiliary gas pressure is 50-60psi, such as 50psi or 60 psi;
l) in the detection condition of the tandem mass spectrum, the declustering voltage is 30-50V, preferably 40V;
m) the detection condition of the tandem mass spectrum, the collision energy is 10-20V, and is preferably 15V.
In certain embodiments of the first aspect of the present invention, the method comprises one or more of the following a) to G):
A) the sample is an essence sample, preferably an essence sample for tobacco;
B) in the step (1), the suitable solvent is absolute methanol;
C) in the step (1), the ratio of the impregnated material to the impregnated;
D) in the step (1), the impregnation is carried out under the ultrasonic condition, and the impregnation time is 15-60 minutes; preferably, the time of immersion is 20-50 minutes, such as 30 minutes, 40 minutes or 45 minutes;
E) in the step (1), the dipping temperature is normal temperature, such as 20-45 ℃, 25 ℃, 30 ℃ and 35 ℃;
F) in the step (1), the solid-liquid separation mode is filtration; preferably, filtration is performed with an organic filter membrane; more preferably, the pore size of the organic filter is 0.1-0.5 μm, e.g. 0.22 μm;
G) in the step (3), quantification is performed by adopting an external standard method.
The second aspect of the present invention relates to a kit comprising: anhydrous methanol, organic filter membrane, C18 chromatographic column, acetonitrile and ammonium acetate solution containing acetic acid.
In certain embodiments of the second aspect of the present invention, the kit further comprises a citronellal standard.
In certain embodiments of the second aspect of the invention, the kit comprises one or more of the following 1) to 5):
1) the pore size of the organic filter membrane is 0.1-0.5 μm, such as 0.2-0.3 μm;
2) the C18 chromatographic column is a Philomen C18 chromatographic column with the specification of 50mm × 2.1.1 mm.d., and the particle size of 2.6 mu m;
3) the molar concentration of ammonium acetate in the ammonium acetate solution is 1-10mmoL/L, preferably 2-8mmoL/L, such as 3mmoL/L, 4mmoL/L, 5mmoL/L, 6mmoL/L, 7mmoL/L or 9 mmoL/L;
4) the volume percentage content of acetic acid in the ammonium acetate solution is 0.05% (v/v) to 0.5% (v/v), preferably 0.1% (v/v) to 0.4% (v/v), such as 0.06% (v/v), 0.1% (v/v), 0.2% (v/v), 0.3% (v/v), 0.45% (v/v);
5) the citronellal standard substance is of a grade higher than analytical purity.
A third aspect of the invention relates to the use of a kit according to any one of the second aspects of the invention for the determination of citronellal in a sample.
In certain embodiments of the third aspect of the present invention, the sample is a flavour sample, preferably a tobacco flavour sample.
Unless otherwise specified, the terms of the present invention are defined as follows:
the term "leaching" refers to the entire process of a solvent entering the tissue cells of a feedstock, dissolving or dispersing the components to be extracted therein to become a leachate.
The term "impregnation" belongs to one of the common extraction methods, and refers to an operation of soaking a raw material with a solvent to dissolve a component to be extracted in the raw material into the solvent; wherein "leaching" is as defined above.
The term "tobacco flavor" includes tobacco flavors and tobacco flavors. Wherein, the tobacco flavor is a flavor which can improve or enhance the aroma or the taste of the tobacco products independently or after being blended; the tobacco essence is an additive of a tobacco product, which is prepared by adding more than two tobacco flavors into auxiliary materials and solvents according to a certain proportion, is specially used for flavoring and correcting the taste of various tobacco products, and can generate fragrance and taste during smoking. The flavors for tobacco include, but are not limited to, flavors for chewing tobacco, flavors for snuff, flavors for cigar, and flavors for cigarette, depending on the type of tobacco product.
The term "liquid chromatography-tandem mass spectrometry" refers to the combination of liquid chromatography with multi-stage tandem mass spectrometry, most commonly liquid chromatography with two-stage tandem mass spectrometry (LC-MS/MS).
The invention has the following beneficial effects:
the determination method of the invention can rapidly and accurately determine the content of citronellal in the tobacco flavor and fragrance, and has good reproducibility and high recovery rate.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the embodiments of the present disclosure taken in conjunction with the accompanying drawings, in which
FIG. 1 is a chromatogram of a standard solution at a concentration of 1.0. mu.g/mL in example 1;
FIG. 2 is a chromatogram of the sample solution of example 1;
FIG. 3 is a mass spectrum of a sample solution in example 1;
FIG. 4 is a standard curve measured from a series of standard solutions in example 1;
fig. 5 is a chromatogram of the sample solution in the comparative example.
Detailed Description
The materials and reagents used in the following examples, comparative examples and test examples were as follows:
citronellal (analytically pure): purchased from carbofuran technologies, inc;
anhydrous methanol: the purity is more than or equal to 99.5 percent (w/w).
Example 1 citronellal in flavor 1 for tobacco (flavor for cigarette)Determination of the content(1) Preparation of a series of standard solutions: weighing 0.1g citronellal (analytically pure) to the accuracy of 0.0001g, dissolving with anhydrous methanol, transferring to a 1000mL volumetric flask, and fixing the volume with anhydrous methanol to obtain a standard stock solution.
Transferring 0.01mL, 0.05mL, 0.1mL, 0.5mL and 1.0mL of standard stock solutions into different 100mL volumetric flasks respectively, and performing constant volume with anhydrous methanol to obtain a series of standard solutions. The concentrations of citronellal in the series of standard solutions were 0.01. mu.g/mL, 0.05. mu.g/mL, 0.1. mu.g/mL, 0.5. mu.g/mL, and 1.0. mu.g/mL, respectively. The series of standard solutions are stored at 4 ℃ in a dark sealed manner, and when the standard solutions are taken, the standard solutions are placed at normal temperature and can be used after reaching the normal temperature, and the marked lines are made once a week.
(2) Preparation of sample solution: weighing 0.1g of tobacco essence spice 1 (essence spice for cigarettes), placing in a 25mL conical flask, accurately adding 10mL of anhydrous methanol, performing ultrasonic treatment at room temperature for 30 minutes, and filtering with a 0.22 μm organic filter membrane to obtain a sample solution. The sample solution was stored at 4 ℃ in a sealed manner for future use.
(3) Detection and analysis: the series of standard solutions and sample solutions were determined by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Wherein, the detection conditions of the high performance liquid chromatography and the tandem mass spectrometry are as follows;
the detection conditions of the high performance liquid chromatography are that a Philomen C18 liquid chromatographic column with the specification of 50mm × 2.1.1 mm i.d., the particle size of 2.6 mu m, the temperature of the chromatographic column of 30 ℃, the sample injection amount of 10 mu L, the mobile phase A of acetonitrile, the mobile phase B of 5mmoL/L ammonium acetate solution (containing 0.1 percent (v/v) of acetic acid), the flow rate of 0.2mL/min and the elution procedure are shown in the table 1,
TABLE 1
Tandem mass spectrometry detection conditions: triple quadrupole mass spectrometry was used; the ion source is an electrospray ionization source (ESI); the scanning mode is positive ion scanning; the detection mode is multi-reaction monitoring (MRM); the electrospray voltage is 4000V; the ion source temperature is 400 ℃; the auxiliary Gas1 pressure was 60 psi; the auxiliary Gas2 pressure was 50 psi; the declustering voltage (DP) is 40V; the Collision Energy (CE) was 15V.
A qualitative ion pair (m/z) of 155.0>81.1 and/or 155.0> 137.2; the quantitative ion pair (m/z) is 155.0> 81.1.
The chromatogram of the 1.0. mu.g/mL standard solution is shown in FIG. 1; the chromatogram of the sample solution is shown in FIG. 2; the mass spectrum of the sample solution is shown in FIG. 3.
(4) And (4) calculating a result:
the peak areas of the chromatographic peaks in the chromatograms of the series of standard solutions are used for carrying out regression analysis on the corresponding concentrations of the chromatographic peaks, the obtained standard curve is shown in figure 4, and the regression equation and the correlation coefficient of the standard curve are shown in table 2.
TABLE 2
Substituting the peak area of the citronellal chromatographic peak in the chromatogram of the sample solution shown in figure 2 into a standard curve to obtain the concentration of citronellal in the sample solution, and calculating according to the following formula to obtain the content of citronellal in the tobacco flavor 1;
m＝(A×S)/n
wherein:
m is the content of citronellal (mu g/g) in the essence and spice for cigarettes;
a-the concentration of citronellal in the sample solution (μ g/mL);
s-volume of sample solution (mL);
and n, weighing the mass (g) of the tobacco essence perfume.
As a result: the content of citronellal in the tobacco flavor 1 is 14.6 mu g/g.
Example 2 determination of citronellal content in essence spice for cigarette 2 (essence spice for cigar)
(1) The preparation of the series of standard solutions was the same as in example 1.
(2) Preparation of sample solution: weighing 0.1g of tobacco essence spice 2 (cigar essence spice), placing in a 25mL conical flask, accurately adding 10mL of anhydrous methanol, performing ultrasonic treatment at room temperature for 30 min, and filtering with 0.22 μm organic filter membrane to obtain sample solution. The sample solution was stored at 4 ℃ in a sealed manner for future use.
(3) Detection and analysis: the series of standard solutions and sample solutions were determined by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Wherein, the detection conditions of the high performance liquid chromatography and the tandem mass spectrometry are the same as those in the example 1.
A qualitative ion pair (m/z) of 155.0>81.1 and/or 155.0> 137.2; the quantitative ion pair (m/z) is 155.0> 81.1.
(4) And (4) calculating a result: the peak areas of chromatographic peaks in the chromatograms of the series of standard solutions are used for carrying out regression analysis on the corresponding concentrations of the chromatographic peaks, and the obtained regression equation and the related coefficients are the same as those in the example 1.
Substituting the peak area of the citronellal chromatographic peak in the chromatogram of the sample solution into a regression equation to obtain the concentration of citronellal in the sample solution, and calculating according to the formula in the embodiment 1 to obtain the content of citronellal in the tobacco flavor and fragrance 2.
As a result: the content of citronellal in the tobacco flavor and fragrance 2 is 10.5 mug/g.
EXAMPLE 3 determination of citronellal content in tobacco flavor 3 (chewing tobacco flavor)(1) The preparation of the series of standard solutions was the same as in example 1.
(2) Preparation of sample solution: 0.1g of tobacco flavor 3 (chewing tobacco flavor) is weighed and placed in a 25mL conical flask, 10mL of anhydrous methanol is accurately added, ultrasonic treatment is carried out for 30 minutes at room temperature, and a sample solution is obtained after filtration by using a 0.22 mu m organic filter membrane. The sample solution was stored at 4 ℃ in a sealed manner for future use.
(3) Detection and analysis: and respectively measuring the series of standard solutions and the sample solution by adopting high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Wherein, the detection conditions of the high performance liquid chromatography and the tandem mass spectrometry are the same as those in example 1.
A qualitative ion pair (m/z) of 155.0>81.1 and/or 155.0> 137.2; the quantitative ion pair (m/z) is 155.0> 81.1.
(4) And (4) calculating a result: the peak areas of chromatographic peaks in the chromatograms of the series of standard solutions are used for carrying out regression analysis on the corresponding concentrations of the chromatographic peaks, and the obtained regression equation and the related coefficients are the same as those in the example 1.
Substituting the peak area of the citronellal chromatographic peak in the chromatogram of the sample solution into a regression equation to obtain the concentration of citronellal in the sample solution, and calculating according to the formula in the embodiment 1 to obtain the content of citronellal in the tobacco flavor 3.
As a result: the content of citronellal in the tobacco flavor and fragrance 3 is 11.3 mug/g.
Example 4 measurement of citronellal content in tobacco flavor 4 (flavor for snuff)(1) The preparation of the series of standard solutions was the same as in example 1.
(2) Preparation of sample solution: 0.1g of tobacco flavor 4 (for snuff) is weighed out and placed in a 25mL conical flask, 10mL of anhydrous methanol is accurately added, ultrasonic treatment is carried out for 30 minutes at room temperature, and a sample solution is obtained after filtration by using a 0.22 mu m organic filter membrane. The sample solution was stored at 4 ℃ in a sealed manner for future use.
(3) Detection and analysis: and respectively measuring the series of standard solutions and the sample solution by adopting high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Wherein, the detection conditions of the high performance liquid chromatography and the tandem mass spectrometry are the same as those in example 1.
A qualitative ion pair (m/z) of 155.0>81.1 and/or 155.0> 137.2; the quantitative ion pair (m/z) is 155.0> 81.1.
(4) And (4) calculating a result: the peak areas of chromatographic peaks in the chromatograms of the series of standard solutions are used for carrying out regression analysis on the corresponding concentrations of the chromatographic peaks, and the obtained regression equation and the related coefficients are the same as those in the example 1.
Substituting the peak area of the citronellal chromatographic peak in the chromatogram of the sample solution into a regression equation to obtain the concentration of citronellal in the sample solution, and calculating according to the formula in the embodiment 1 to obtain the content of citronellal in the tobacco flavor and fragrance 4.
As a result: the content of citronellal in the tobacco flavor and fragrance 4 is 9.7 mu g/g.
Example 5 reproducibility and accuracy of the method
(1) The preparation of the series of standard solutions was the same as in example 1.
(2) Preparation of a labeling sample solution: three portions of the tobacco flavor 1 are weighed as samples, each portion is 0.1g, 0.01mL, 0.02mL and 0.05mL of the standard stock solution in the embodiment 1 are respectively added into the three portions of the samples to obtain a labeled sample, and then, a labeled sample solution is prepared according to the method in the step (2) in the embodiment 1.
(3) Detection and analysis: and (3) measuring a series of standard solutions and standard sample solutions by adopting high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Wherein, the detection conditions of the high performance liquid chromatography and the tandem mass spectrometry are the same as those in the example 1, and each labeled sample solution is detected for 6 times.
A qualitative ion pair (m/z) of 155.0>81.1 and/or 155.0> 137.2; the quantitative ion pair (m/z) is 155.0> 81.1.
(4) And (4) calculating a result: the peak areas of chromatographic peaks in the chromatograms of the series of standard solutions are used for carrying out regression analysis on the corresponding concentrations of the chromatographic peaks, and the obtained regression equation and the related coefficients are the same as those in the example 1.
Substituting the peak area of the citronellal chromatographic peak in the chromatogram of the standard sample solution into a regression equation to obtain the concentration of citronellal in the standard sample solution, calculating according to the formula in the embodiment 1 to obtain the content of citronellal in the standard sample, and further calculating to obtain the standard recovery rate, the average standard recovery rate and the RSD of citronellal in the tobacco flavor 1, wherein the results are shown in Table 3.
Table 3 recovery and repeatability of citronellal in flavor and fragrance for tobacco 1 (n ═ 6)
As can be seen from Table 3, on the three standard adding levels, the recovery rate of citronellal in the tobacco flavor and fragrance 1 is between 90.1% and 97.3%, and the relative standard deviation of the sample test result is less than 5%, which indicates that the standard adding recovery rate of the method is high, the accuracy is high, and the repeatability is good.
Influence of comparative example elution procedure on determination of citronellal content in tobacco flavor and fragrance
And (3) measuring the content of citronellal in the tobacco flavor 1 (the flavor for cigarettes). The procedure was the same as in example 1 except that the elution procedure of the high performance liquid chromatography was as shown in Table 4.
TABLE 4
The chromatogram obtained for the sample solution is shown in FIG. 5.
As can be seen by comparing FIG. 2 with FIG. 5, in the chromatogram of the comparative example, the citronellal chromatographic peak and the impurity chromatographic peak can not be separated, and impurity interference exists, so that the content of citronellal can not be accurately determined. The determination method of the invention has high separation degree of citronellal and impurities, and can more accurately quantify the content of citronellal in the tobacco flavor and fragrance.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (14)
1. A method for measuring citronellal in a tobacco flavor sample comprises the following steps:
(1) impregnating an essence and spice sample for cigarettes by using anhydrous methanol, and carrying out solid-liquid separation to obtain an extracting solution;
(2) detecting the extracting solution obtained in the step (1) by adopting liquid chromatography-tandem mass spectrometry to obtain a detection result;
(3) qualitatively analyzing and/or quantitatively calculating citronellal in the sample according to the detection result obtained in the step (2);
in the step (2), in the detection conditions of the liquid chromatography, the mobile phase consists of a mobile phase A and a mobile phase B, wherein the mobile phase A is acetonitrile, the mobile phase B is an ammonium acetate solution containing acetic acid, and the molar concentration of ammonium acetate in the mobile phase B is 1-10mmoL/L, and the elution procedure is shown in the following table 1:
TABLE 1
；
In the step (2), in the detection conditions of the tandem mass spectrum, the mass spectrum is a triple quadrupole mass spectrum, the electrospray voltage is 3500-.
2. The method according to claim 1, wherein in the step (2), the detection condition of the liquid chromatography is that the molar concentration of ammonium acetate in the mobile phase B is 2-8 mmoL/L.
3. The method according to claim 1, wherein in the step (2), the detection condition of the liquid chromatography comprises that the content of acetic acid in the mobile phase B is 0.05% (v/v) to 0.5% (v/v) by volume.
4. The method according to claim 1, wherein in the step (2), the detection condition of the liquid chromatography comprises that the content of acetic acid in the mobile phase B is 0.08% (v/v) to 0.4% (v/v) by volume.
5. The method of claim 1, wherein step (2) further comprises one or more of the following a) through k):
a) the liquid chromatography is high performance liquid chromatography;
b) in the detection conditions of the liquid chromatography, a chromatographic column is a C18 chromatographic column;
c) in the detection condition of the liquid chromatogram, the temperature of a chromatographic column is 20-40 ℃;
d) in the detection condition of the liquid chromatogram, the flow rate is 0.1-1 mL/min;
e) in the detection condition of the tandem mass spectrum, an ion source is an electrospray ionization source;
f) in the detection condition of the tandem mass spectrum, the scanning mode is positive ion scanning;
g) in the detection condition of the tandem mass spectrum, the detection mode is multi-reaction monitoring;
h) in the detection condition of the tandem mass spectrum, the electrospray voltage is 4000V;
i) in the detection condition of the tandem mass spectrum, the temperature of an ion source is 400 ℃;
j) in the detection condition of the tandem mass spectrum, the auxiliary air pressure is 50-60 psi;
k) in the detection condition of the tandem mass spectrum, the declustering voltage is 30-50V.
6. The method of claim 5, wherein in item b), the column is a Firmor C18 column, having a size of 50mm × 2.1.1 mm.d., 2.6 μm.
7. The method of claim 5, wherein in item c), the column temperature is from 28 ℃ to 32 ℃.
8. The method of claim 5, wherein in item d), the flow rate is 0.1-0.5 mL/min.
9. The method of claim 5, wherein in item k), the declustering voltage is 40V.
10. The method according to any one of claims 1 to 9, comprising one or more of the following a) to E):
A) in the step (1), the ratio of the impregnated material to the impregnated liquid is 1-30 mg/mL;
B) in the step (1), the impregnation is carried out under the ultrasonic condition, and the impregnation time is 15-60 minutes;
C) in the step (1), the dipping temperature is normal temperature;
D) in the step (1), the solid-liquid separation mode is filtration;
E) in the step (3), quantification is performed by adopting an external standard method.
11. The method according to claim 10, wherein in item a), the impregnation in step (1) is carried out at a feed-to-liquid ratio of 4 to 20 mg/mL.
12. The method according to claim 10, wherein in item B), the time for the immersion in step (1) is 20 to 50 minutes.
13. The process of claim 10, wherein in item D), filtration is carried out using an organic filter membrane.
14. The method of claim 13, wherein the pore size of the organic filter is 0.1-0.5 μm.
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