CN110554119A - Quantitative detection method for tree moss aroma phenolic substances - Google Patents
Quantitative detection method for tree moss aroma phenolic substances Download PDFInfo
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Abstract
the invention discloses a method for quantitatively detecting tree moss aroma phenolic substances in tree moss aroma plants or extracts, which adopts an ultra-high performance liquid chromatography-tandem mass spectrometry combined method to detect the tree moss aroma phenolic substances in the tree moss aroma plants or extracts, and the method comprises the steps of collecting 0.1 ~ 2g of the tree moss aroma plants or extracts by using a sample tube, adding 1 ~ 10mL of water, fully oscillating for 10 ~ 30min, taking 1 ~ 2mL of an extraction solution into a chromatographic bottle, quickly sealing, and analyzing by using a high performance liquid chromatography-tandem mass spectrometry combined instrument to quantify an external standard method.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method special for detecting tree moss phenolic substances in tree moss plants or extracts.
Background
the tree moss (Everniafurfuraceae) belongs to Usneaceae (Usneaceae) plant of tree moss (Ramalina), is mainly distributed in Yunnan, Guizhou and other places, due to complex terrain and variable climate, the formed tree moss varieties are various, namely bush flower (Ramalinafastigiata), schizophyllan (Ramalinaminuscula), pseudodendron (Ramalinacommista) and the like, the surface is mainly grey green or dark green, the chemical components are different in type and content, industrially, active ingredients in the tree moss are mainly extracted by hydrocarbon series solvents such as petroleum ether or benzene and the like to obtain a tree moss extract, and after wax and other impurities are further processed by ethanol, the tree moss clean oil can be obtained, the tree moss extract is unique and natural in fragrance, rich in resin smell, good in penetrability and lasting in fragrance, is a natural moss spice which is important, is widely applied to the industries such as cigarettes, cosmetics and the like at present, and researches discover that phenolic compounds directly or indirectly contribute to the tree moss fragrance, such as 3, 5-dihydroxytoluene (also 3, 5-toluene or phenol).
The research on the tree moss aroma phenolic substances in the tree moss aroma plants or extracts is beneficial to understanding and mastering the source and the content of the tree moss aroma components, and the control capability of the autonomous flavoring process on the quality of spice raw materials and products is improved. The content of tree moss phenolic substances in the tree moss fragrant plant or extract is low, the interference during detection is large, the requirement on sample pretreatment is high, and a quantitative detection method for the tree moss phenolic substances in the tree moss fragrant plant or extract is not reported at present, so that the method special for detecting the tree moss phenolic substances in the tree moss fragrant plant or extract is particularly important.
Disclosure of Invention
The invention aims to provide a method for detecting tree moss phenolic substances in tree moss plants or extracts, which has the advantages of rapidness, accuracy, simple operation and the like.
Collecting 0.1 ~ 2g of tree moss fragrant plants or extracts by using a sample tube, adding 1 ~ 10mL of water, fully oscillating for 10 ~ 30min, taking 1 ~ 2mL of extract liquor to a chromatographic bottle, quickly sealing, analyzing by an ultra performance liquid chromatography-tandem mass spectrometer, and quantifying according to component peak areas;
The liquid chromatogram condition is that the chromatographic column is a Waters ACQUITY UPLC HSS T3 column with 1.8 μm and 2.1 × 50mm, the mobile phase adopts methanol/0.1 ~ 0.5.5% formic acid aqueous solution, wherein 0min methanol/0.1 ~ 0.5% formic acid aqueous solution =5/95, 2min methanol/0.1 ~ 0.5% formic acid aqueous solution =90/10, 4min methanol/0.1 ~ 0.5.5% formic acid aqueous solution =5/95, 6min methanol/0.1 ~ 0.5% formic acid aqueous solution =5/95, the column temperature is 30 ~ 45 ℃, the flow rate is 0.1 ~ 0.4mL/min, and the sample feeding amount is 2 ~ 6 μ L;
The mass spectrum conditions comprise that an 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 3500 ~ 5500V, the ion source temperature is 350 ~ 650 ℃, the auxiliary Gas Gas1 pressure is 0.206 ~ 0.345MPa, the auxiliary Gas Gas2 pressure is 0.414 ~ 0.517.517 MPa, the ion monitoring mode is selected, and the ion selection parameters are as follows:
The quantitative ion pair of 3, 4-dimethylphenol is 122.1/107.2, the DP voltage is 21 ~ 28V, the CE voltage is 20 ~ 27V, the CXP voltage is 1.0 ~ 1.6.6V, the qualitative ion pair is 122.1/71.1, the DP voltage is 23 ~ 30V, the CE voltage is 28 ~ 33V, and the CXP voltage is 0.9 ~ 1.6.6V;
The quantitative ion pair of the 3-methoxy-5-methylphenol is 138.2/109.2, the DP voltage is 10 ~ 18V, the CE voltage is 10 ~ 16V, and the CXP voltage is 1.8 ~ 2.5.5V, the qualitative ion pair is 138.2/107.1, the DP voltage is 8 ~ 15V, the CE voltage is 20 ~ 25V, and the CXP voltage is 1.8 ~ 2.3.3V;
the quantitative ion pair of 3-methoxy-2, 5, 6-trimethylphenol is 166.2/151.2, the DP voltage is 14 ~ 18V, the CE voltage is 18 ~ 22V, the CXP voltage is 2.0 ~ 2.5.5V, the qualitative ion pair is 166.2/91.1, the DP voltage is 11 ~ 16V, the CE voltage is 16 ~ 22V, and the CXP voltage is 1.4 ~ 1.9.9V;
the quantitative ion pair of the 3, 5-dihydroxytoluene is 124.2/95.2, the DP voltage is 20 ~ 24V, the CE voltage is 22 ~ 26V, the CXP voltage is 2.2 ~ 2.7.7V, the qualitative ion pair is 124.2/59.1, the DP voltage is 19 ~ 24V, the CE voltage is 22 ~ 27V, and the CXP voltage is 1.8 ~ 2.2V;
The quantitative ion pair of the 2, 5-dihydroxytoluene is 124.2/123.2, the DP voltage is 20 ~ 25V, the CE voltage is 14 ~ 17V, the CXP voltage is 1.3 ~ 1.8V, the qualitative ion pair is 124.2/67.2, the DP voltage is 19 ~ 25V, the CE voltage is 30 ~ 34V, and the CXP voltage is 2.2 ~ 2.6.6V;
The quantitative ion pair of 5-methoxy-2, 3-xylenol is 152.1/137.2, the DP voltage is 12 ~ 17V, the CE voltage is 15 ~ 20V, the CXP voltage is 2.4 ~ 2.8.8V, the qualitative ion pair is 152.1/77.1, the DP voltage is 16 ~ 20V, the CE voltage is 13 ~ 17V, and the CXP voltage is 2.2 ~ 2.6.6V;
the quantitative ion pair of 2, 5-dimethyl-1, 4-benzenediol is 138.2/123.1, the DP voltage is 23 ~ 27V, the CE voltage is 18 ~ 22V, the CXP voltage is 2.4 ~ 2.9V, the qualitative ion pair is 138.2/95.1, the DP voltage is 22 ~ 26V, the CE voltage is 33 ~ 38V, and the CXP voltage is 2.5 ~ 2.9.9V.
The method for detecting the tree moss phenolic substances in the tree moss plants or the tree moss extracts has the following positive effects:
(1) the method has simple steps, can carry out sample injection analysis only after extraction, has simple treatment steps and is easy to popularize;
(2) The method has high accuracy, greatly reduces the loss of an analyte in the purification transfer process, increases the accuracy of the analysis process, and has the advantages that the relative standard deviation of 3, 4-dimethylphenol is between 2.68 percent ~ 3.54.54 percent, the relative standard deviation of 3-methoxy-5-methylphenol is between 2.30 percent ~ 4.82.82 percent, the relative standard deviation of 3-methoxy-2, 5, 6-trimethylphenol is between 1.26 percent ~ 3.69.69 percent, the relative standard deviation of 3, 5-dihydroxytoluene is between 2.13 percent ~ 4.98.98 percent, the relative standard deviation of 2, 5-dihydroxytoluene is between 1.16 percent ~ 4.02.02 percent, the relative standard deviation of 5-methoxy-2, 3-dimethylphenol is between 2.56 percent ~ 4.64.64 percent, and the relative standard deviation of 2, 5-dimethyl-1, 4-benzenediol is between 1.32 percent ~ 3.69.69 percent;
(3) The method is environment-friendly, improves the analysis accuracy and reduces the pollution to the environment.
The method is used for detecting the tree moss phenolic substances in the tree moss plants or extracts, and has the advantages of rapidness, accuracy, simplicity in operation and the like.
Drawings
FIG. 1 is a liquid chromatogram of Moss phenolic compounds in Moss plant extract;
Wherein the chromatographic peak with the retention time of 0.85 min is 3, 4-dimethylphenol, the chromatographic peak with the retention time of 1.36 min is 3-methoxy-5-methylphenol, the chromatographic peak with the retention time of 1.59 min is 3-methoxy-2, 5, 6-trimethylphenol, the chromatographic peak with the retention time of 2.08 min is 3, 5-dihydroxytoluene, the chromatographic peak with the retention time of 2.72 min is 2, 5-dihydroxytoluene, the chromatographic peak with the retention time of 3.25 min is 5-methoxy-2, 3-dimethylphenol, and the chromatographic peak with the retention time of 3.61min is 2, 5-dimethyl-1, 4-benzenediol.
Detailed Description
The present invention will be described in further detail with reference to examples.
it will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available by purchase.
Example 1
Collecting 0.1 g of the plant extract (extractum) of the tree moss incense by using a sample tube, adding 1mL of water, fully oscillating for 10min, taking 1mL of extract to a chromatographic bottle, quickly sealing, analyzing by an ultra-high performance liquid chromatography-tandem mass spectrometer, and quantifying according to peak areas of components;
the liquid chromatogram conditions are as follows: the chromatographic column is a Waters ACQUITY UPLC HSS T3 column with the diameter of 1.8 μm and the diameter of 2.1 × 50mm, and the mobile phase adopts methanol/0.1% formic acid aqueous solution, wherein 0min methanol/0.1 formic acid aqueous solution =5/95, 2min methanol/0.1 formic acid aqueous solution =90/10, 4min methanol/0.1 formic acid aqueous solution =5/95, 6min methanol/0.1 formic acid aqueous solution =5/95, the column temperature is 30 ℃, the flow rate is 0.1mL/min, and the sample feeding amount is 2 μ L;
The mass spectrum conditions are as follows: 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 3500V, the ion source temperature is 350 ℃, the pressure of auxiliary Gas Gas1 is 0.206 MPa, and the pressure of auxiliary Gas Gas2 is 0.414 MPa; selecting an ion monitoring mode, wherein the ion selection parameters are as follows: the quantitative ion pair of 3, 4-dimethylphenol is 122.1/107.2, the DP voltage is 21V, the CE voltage is 20V, and the CXP voltage is 1.0V; the qualitative ion pair is 122.1/71.1, the DP voltage is 23V, the CE voltage is 28V, and the CXP voltage is 0.9V; the quantitative ion pair of the 3-methoxy-5-methylphenol is 138.2/109.2, the DP voltage is 10V, the CE voltage is 10V, and the CXP voltage is 1.8V; the qualitative ion pair is 138.2/107.1, the DP voltage is 8V, the CE voltage is 20V, and the CXP voltage is 1.8V; the quantitative ion pair of 3-methoxy-2, 5, 6-trimethylphenol is 166.2/151.2, the DP voltage is 14V, the CE voltage is 18V, and the CXP voltage is 2.0V; the qualitative ion pair is 166.2/91.1, the DP voltage is 11V, the CE voltage is 16V, and the CXP voltage is 1.4V; the quantitative ion pair of the 3, 5-dihydroxytoluene is 124.2/95.2, the DP voltage is 20V, the CE voltage is 22V, and the CXP voltage is 2.2V; the qualitative ion pair is 124.2/59.1, the DP voltage is 19V, the CE voltage is 22V, and the CXP voltage is 1.8V; the quantitative ion pair of the 2, 5-dihydroxytoluene is 124.2/123.2, the DP voltage is 20V, the CE voltage is 14V, and the CXP voltage is 1.3V; the qualitative ion pair is 124.2/67.2, the DP voltage is 19V, the CE voltage is 30V, and the CXP voltage is 2.2V; the quantitative ion pair of the 5-methoxy-2, 3-xylenol is 152.1/137.2, the DP voltage is 12V, the CE voltage is 15V, and the CXP voltage is 2.4V; the qualitative ion pair is 152.1/77.1, the DP voltage is 16V, the CE voltage is 13V, and the CXP voltage is 2.2V; the quantitative ion pair of the 2, 5-dimethyl-1, 4-benzenediol is 138.2/123.1, the DP voltage is 23V, the CE voltage is 18V, and the CXP voltage is 2.4V; the qualitative ion pair was 138.2/95.1, DP voltage 22V, CE voltage 33V, and CXP voltage 2.5V (see FIG. 1).
The average of 5 replicates of 3, 4-dimethylphenol was 2.92ng/mg with a relative standard deviation of 2.68% as described above; the average value of 5-time parallel determination results of the 3-methoxy-5-methylphenol is 0.76ng/mg, and the relative standard deviation is 2.30%; the average value of 5 times of parallel determination results of the 3-methoxy-2, 5, 6-trimethylphenol is 0.23ng/mg, and the relative standard deviation is 1.26 percent; the average of 5 replicates of 3, 5-dihydroxytoluene was 310.17ng/mg with a relative standard deviation of 2.13%; the average of 5 replicates of 2, 5-dihydroxytoluene was 0.21ng/mg with a relative standard deviation of between 1.16%; the average value of 5-time parallel determination results of the 5-methoxy-2, 3-xylenol is 2.56ng/mg, and the relative standard deviation is 2.56%; the average of 5 replicates of 2, 5-dimethyl-1, 4-benzenediol was 6.32ng/mg with a relative standard deviation of 1.32%.
example 2
Collecting 1 g of tree moss fragrant plants by using a sample tube, adding 5 mL of water, fully oscillating for 20 min, taking 1.5 mL of extract liquid to a chromatographic bottle, quickly sealing, analyzing by an ultra performance liquid chromatography-tandem mass spectrometer, and quantifying according to peak areas of components;
The liquid chromatogram conditions are as follows: the chromatographic column is a Waters ACQUITY UPLC HSS T3 column with the diameter of 1.8 μm and the diameter of 2.1 × 50mm, and the mobile phase adopts methanol/0.5% formic acid aqueous solution, wherein 0min methanol/0.5% formic acid aqueous solution =5/95, 2min methanol/0.5% formic acid aqueous solution =90/10, 4min methanol/0.5% formic acid aqueous solution =5/95, 6min methanol/0.5% formic acid aqueous solution 5/95, the column temperature is 40 ℃, the flow rate is 0.2mL/min, and the sample injection amount is 4 μ L;
The mass spectrum conditions are as follows: 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 5000V, the ion source temperature is 500 ℃, the pressure of auxiliary Gas Gas1 is 0.345MPa, and the pressure of auxiliary Gas Gas2 is 0.414 MPa; selecting an ion monitoring mode, wherein the ion selection parameters are as follows: the quantitative ion pair of 3, 4-dimethylphenol is 122.1/107.2, the DP voltage is 24V, the CE voltage is 23V, and the CXP voltage is 1.3V; the qualitative ion pair is 122.1/71.1, the DP voltage is 26V, the CE voltage is 29V, and the CXP voltage is 1.3V; the quantitative ion pair of the 3-methoxy-5-methylphenol is 138.2/109.2, the DP voltage is 13V, the CE voltage is 15V, and the CXP voltage is 1.9V; the qualitative ion pair is 138.2/107.1, the DP voltage is 10V, the CE voltage is 22V, and the CXP voltage is 2.0V; the quantitative ion pair of the 3-methoxy-2, 5, 6-trimethylphenol is 166.2/151.2, the DP voltage is 16V, the CE voltage is 20V, and the CXP voltage is 2.3V; the qualitative ion pair is 166.2/91.1, the DP voltage is 15V, the CE voltage is 20V, and the CXP voltage is 1.5V; the quantitative ion pair of the 3, 5-dihydroxytoluene is 124.2/95.2, the DP voltage is 22V, the CE voltage is 25V, and the CXP voltage is 2.5V; the qualitative ion pair is 124.2/59.1, the DP voltage is 23V, the CE voltage is 25V, and the CXP voltage is 2.0V; the quantitative ion pair of the 2, 5-dihydroxytoluene is 124.2/123.2, the DP voltage is 23V, the CE voltage is 15V, and the CXP voltage is 1.6V; the qualitative ion pair is 124.2/67.2, the DP voltage is 20V, the CE voltage is 32V, and the CXP voltage is 2.3V; the quantitative ion pair of the 5-methoxy-2, 3-xylenol is 152.1/137.2, the DP voltage is 15V, the CE voltage is 16V, and the CXP voltage is 2.6V; the qualitative ion pair is 152.1/77.1, the DP voltage is 18V, the CE voltage is 15V, and the CXP voltage is 2.5V; the quantitative ion pair of the 2, 5-dimethyl-1, 4-benzenediol is 138.2/123.1, the DP voltage is 25V, the CE voltage is 19V and the CXP voltage is 2.6V; the qualitative ion pair was 138.2/95.1, the DP voltage was 25V, the CE voltage was 35V, and the CXP voltage was 2.8V.
the average of 5 replicates of 3, 4-dimethylphenol was 0.28ng/mg with a relative standard deviation of 2.84% as described above; the average value of 5-time parallel determination results of the 3-methoxy-5-methylphenol is 0.38ng/mg, and the relative standard deviation is 3.28%; the average value of 5 times of parallel determination results of the 3-methoxy-2, 5, 6-trimethylphenol is 0.12ng/mg, and the relative standard deviation is 3.62 percent; the average of 5 replicates of 3, 5-dihydroxytoluene was 14.25ng/mg with a relative standard deviation of 3.56%; the average of 5 replicates of 2, 5-dihydroxytoluene was 0.18ng/mg with a relative standard deviation of 3.89%; the average value of 5-time parallel determination results of the 5-methoxy-2, 3-xylenol is 0.21ng/mg, and the relative standard deviation is 3.56%; the average of 5 replicates of 2, 5-dimethyl-1, 4-benzenediol was 1.23ng/mg with a relative standard deviation of 2.69%.
Example 3
Collecting 2g of tree moss plant extract (neat oil) by using a sample tube, adding 10mL of water, fully oscillating for 30min, taking 2mL of extract to a chromatographic bottle, rapidly sealing, analyzing by an ultra performance liquid chromatography-tandem mass spectrometer, and quantifying according to component peak areas;
the liquid chromatogram conditions are as follows: the chromatographic column is a Waters ACQUITY UPLC HSS T3 column with a diameter of 1.8 μm and a diameter of 2.1 × 50mm, and the mobile phase is methanol/0.3% aqueous formic acid, wherein 0min methanol/0.3% aqueous formic acid =5/95, 2min methanol/0.3% aqueous formic acid =90/10, 4min methanol/0.3% aqueous formic acid =5/95, 6min methanol/0.3% aqueous formic acid =5/95, the column temperature is 45 deg.C, the flow rate is 0.4mL/min, and the sample introduction amount is 6 μ L.
The mass spectrum conditions are as follows: 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 5500V, the ion source temperature is 650 ℃, the pressure of auxiliary Gas Gas1 is 0.345MPa, and the pressure of auxiliary Gas Gas2 is 0.517 MPa; selecting an ion monitoring mode, wherein the ion selection parameters are as follows: the quantitative ion pair of 3, 4-dimethylphenol is 122.1/107.2, the DP voltage is 28V, the CE voltage is 27V, and the CXP voltage is 1.6V; the qualitative ion pair is 122.1/71.1, the DP voltage is 30V, the CE voltage is 33V, and the CXP voltage is 1.6V; the quantitative ion pair of the 3-methoxy-5-methylphenol is 138.2/109.2, the DP voltage is 18V, the CE voltage is 16V, and the CXP voltage is 2.5V; the qualitative ion pair is 138.2/107.1, the DP voltage is 15V, the CE voltage is 25V, and the CXP voltage is 2.3V; the quantitative ion pair of the 3-methoxy-2, 5, 6-trimethylphenol is 166.2/151.2, the DP voltage is 18V, the CE voltage is 22V, and the CXP voltage is 2.5V; the qualitative ion pair is 166.2/91.1, the DP voltage is 16V, the CE voltage is 22V, and the CXP voltage is 1.9V; the quantitative ion pair of the 3, 5-dihydroxytoluene is 124.2/95.2, the DP voltage is 24V, the CE voltage is 26V, and the CXP voltage is 2.7V; the qualitative ion pair is 124.2/59.1, the DP voltage is 24V, the CE voltage is 27V, and the CXP voltage is 2.2V; the quantitative ion pair of the 2, 5-dihydroxytoluene is 124.2/123.2, the DP voltage is 25V, the CE voltage is 17V, and the CXP voltage is 1.8V; the qualitative ion pair is 124.2/67.2, the DP voltage is 25V, the CE voltage is 34V, and the CXP voltage is 2.6V; the quantitative ion pair of the 5-methoxy-2, 3-xylenol is 152.1/137.2, the DP voltage is 17V, the CE voltage is 20V, and the CXP voltage is 2.8V; the qualitative ion pair is 152.1/77.1, the DP voltage is 20V, the CE voltage is 17V, and the CXP voltage is 2.6V; the quantitative ion pair of the 2, 5-dimethyl-1, 4-benzenediol is 138.2/123.1, the DP voltage is 27V, the CE voltage is 22V and the CXP voltage is 2.9V; the qualitative ion pair was 138.2/95.1, the DP voltage was 26V, the CE voltage was 38V, and the CXP voltage was 2.9V.
the average of 5 replicates of 3, 4-dimethylphenol was 2.56ng/mg with a relative standard deviation of 2.33%, as described above; the average value of 5-time parallel determination results of the 3-methoxy-5-methylphenol is 0.72ng/mg, and the relative standard deviation is 3.52 percent; the average value of 5 times of parallel determination results of the 3-methoxy-2, 5, 6-trimethylphenol is 0.19ng/mg, and the relative standard deviation is 3.29 percent; the average of 5 replicates of 3, 5-dihydroxytoluene was 295.16ng/mg with a relative standard deviation of 2.36%; the average of 5 replicates of 2, 5-dihydroxytoluene was 0.21ng/mg with a relative standard deviation of 3.49%; the average value of 5-time parallel determination results of the 5-methoxy-2, 3-xylenol is 2.20ng/mg, and the relative standard deviation is 4.14%; the average of 5 replicates of 2, 5-dimethyl-1, 4-benzenediol was 6.22ng/mg with a relative standard deviation of 3.18%.
the foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. A quantitative detection method of arborvitae scent phenolic substances is characterized in that 0.1 ~ 2g of arborvitae scent plants or extracts is collected by a sample tube, 1 ~ 10mL of water is added, the mixture is fully oscillated for 10 ~ 30min, 1 ~ 2mL of extract liquid is taken to a chromatographic bottle, the mixture is quickly sealed, and the mixture is analyzed by an ultra-high performance liquid chromatography-tandem mass spectrometer, and the quantification is carried out according to the peak areas of the components;
The liquid chromatography conditions were as follows:
The chromatographic column is a Waters ACQUITY UPLC HSS T3 column with 1.8 μm and 2.1 × 50mm, and the mobile phase is methanol/0.1 ~ 0.5.5% aqueous solution of formic acid, wherein 0min methanol/0.1 ~ 0.5% aqueous solution of formic acid =5/95, 2min methanol/0.1 ~ 0.5% aqueous solution of formic acid =90/10, 4min methanol/0.1 ~ 0.5.5% aqueous solution of formic acid =5/95, 6min methanol/0.1 ~ 0.5% aqueous solution of formic acid =5/95, the column temperature is 30 ~ 45 ℃, the flow rate is 0.1 ~ 0.4mL/min, and the sample injection amount is 2 ~ 6 μ L;
the mass spectrum conditions were as follows:
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 3500 ~ 5500V, the ion source temperature is 350 ~ 650 ℃, the auxiliary Gas Gas1 pressure is 0.206 ~ 0.345.345 MPa, the auxiliary Gas Gas2 pressure is 0.414 ~ 0.517.517 MPa, the ion monitoring mode is selected, and the ion selection parameters are as follows:
The quantitative ion pair of 3, 4-dimethylphenol is 122.1/107.2, the DP voltage is 21 ~ 28V, the CE voltage is 20 ~ 27V, the CXP voltage is 1.0 ~ 1.6.6V, the qualitative ion pair is 122.1/71.1, the DP voltage is 23 ~ 30V, the CE voltage is 28 ~ 33V, and the CXP voltage is 0.9 ~ 1.6.6V;
The quantitative ion pair of the 3-methoxy-5-methylphenol is 138.2/109.2, the DP voltage is 10 ~ 18V, the CE voltage is 10 ~ 16V, and the CXP voltage is 1.8 ~ 2.5.5V, the qualitative ion pair is 138.2/107.1, the DP voltage is 8 ~ 15V, the CE voltage is 20 ~ 25V, and the CXP voltage is 1.8 ~ 2.3.3V;
The quantitative ion pair of 3-methoxy-2, 5, 6-trimethylphenol is 166.2/151.2, the DP voltage is 14 ~ 18V, the CE voltage is 18 ~ 22V, the CXP voltage is 2.0 ~ 2.5.5V, the qualitative ion pair is 166.2/91.1, the DP voltage is 11 ~ 16V, the CE voltage is 16 ~ 22V, and the CXP voltage is 1.4 ~ 1.9.9V;
the quantitative ion pair of the 3, 5-dihydroxytoluene is 124.2/95.2, the DP voltage is 20 ~ 24V, the CE voltage is 22 ~ 26V, the CXP voltage is 2.2 ~ 2.7.7V, the qualitative ion pair is 124.2/59.1, the DP voltage is 19 ~ 24V, the CE voltage is 22 ~ 27V, and the CXP voltage is 1.8 ~ 2.2V;
the quantitative ion pair of the 2, 5-dihydroxytoluene is 124.2/123.2, the DP voltage is 20 ~ 25V, the CE voltage is 14 ~ 17V, the CXP voltage is 1.3 ~ 1.8V, the qualitative ion pair is 124.2/67.2, the DP voltage is 19 ~ 25V, the CE voltage is 30 ~ 34V, and the CXP voltage is 2.2 ~ 2.6.6V;
the quantitative ion pair of 5-methoxy-2, 3-xylenol is 152.1/137.2, the DP voltage is 12 ~ 17V, the CE voltage is 15 ~ 20V, the CXP voltage is 2.4 ~ 2.8.8V, the qualitative ion pair is 152.1/77.1, the DP voltage is 16 ~ 20V, the CE voltage is 13 ~ 17V, and the CXP voltage is 2.2 ~ 2.6.6V;
The quantitative ion pair of 2, 5-dimethyl-1, 4-benzenediol is 138.2/123.1, the DP voltage is 23 ~ 27V, the CE voltage is 18 ~ 22V, the CXP voltage is 2.4 ~ 2.9V, the qualitative ion pair is 138.2/95.1, the DP voltage is 22 ~ 26V, the CE voltage is 33 ~ 38V, and the CXP voltage is 2.5 ~ 2.9.9V.
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