Method for detecting ginger in Chinese patent medicine based on high-resolution mass spectrometry technology

Abstract

The invention discloses a method for detecting ginger in a Chinese patent medicine based on a high-resolution mass spectrometry technology, which comprises the following steps: (1) preparation of a reference substance solution: taking a proper amount of a characteristic component hexahydrocurcumin reference substance, precisely weighing, and adding an alcohol reagent for dissolving to obtain the reference substance solution; (2) preparation of a test sample solution: taking a test sample, precisely weighing, and adding an alcohol reagent for extraction to obtain the test sample solution; (3) determination: respectively collecting extracted ion flow chromatograms of the reference substance solution and the test solution by adopting ultra-high performance liquid chromatography combined with triple quadrupole mass spectrometry; if a chromatographic peak corresponding to the hexahydrocurcumin reference substance is detected in the test sample, the test sample contains the ginger, and otherwise, the test sample does not contain the ginger. The method can effectively solve the problem of judging whether the fresh ginger is contained in the Chinese patent medicine, especially the traditional Chinese medicine compound aqueous extract, in actual work, and provides a technical method and basis for fighting against illegal behaviors such as insufficient feeding, non-feeding or illegal feeding of enterprises in compression cost.

Description

Technical Field

[0001] The present invention relates to the technical field of pharmaceutical analysis and detection, and particularly relates to a method for detecting ginger in Chinese patent medicines based on high-resolution mass spectrometry technology. Background Art

[0002] Ginger is the fresh rhizome of Zingiber officinale Rosc. of the Zingiberaceae family and is a commonly used traditional Chinese medicine. The integrity of the raw medicinal materials has been damaged in the finished products of Chinese patent medicines. There may be a possibility that some enterprises cut costs by not using the full amount of raw materials, not using any raw materials, or using raw materials illegally. Due to the lack of effective quality control items and other reasons, inspectors cannot effectively determine whether ginger is contained in Chinese patent medicines. Clinically in traditional Chinese medicine, ginger has the effects of relieving exterior syndrome and dispelling cold, warming the middle-jiao to arrest vomiting, resolving phlegm and relieving cough, and detoxifying fish and crab poisoning. It is commonly used for wind-cold cold, stomach cold vomiting, cold phlegm cough, and fish and crab poisoning. As a complex system in which multiple components interact with multiple targets and work together, the lack of ginger in the formulation may seriously affect the clinical efficacy.

[0003] In addition, the main components contained in ginger are volatile oils, gingerols, etc. However, the traditional application form of ginger in traditional Chinese medicine compound is mostly decocted by water, which results in extremely low contents of these volatile and fat-soluble components in the traditional Chinese medicine compound and makes them difficult to detect, bringing difficulties to the quality detection and supervision of drugs.

[0004] Therefore, it is particularly important to seek an efficient and specific method for detecting ginger in Chinese patent medicines, especially the water extracts of traditional Chinese medicine compounds. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to overcome the technical defects of the background art and provide a method for detecting ginger in Chinese patent medicines based on high-resolution mass spectrometry technology. With the rapid development of mass spectrometry technology, ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) has the advantages of fast analysis speed, high sensitivity and resolution, and has significant advantages in separating and analyzing endogenous components in the complex matrix of traditional Chinese medicine prescriptions. Based on the above situation, the specific component hexahydrocurcumin in the water extract of ginger was screened, and a detection method based on ultra-high performance liquid chromatography combined with triple quadrupole mass spectrometry technology was developed, which can effectively solve the problem of determining whether ginger is contained in Chinese patent medicines, especially the water extracts of traditional Chinese medicine compounds, in actual work, and provide a technical method and basis for cracking down on illegal acts such as enterprises cutting costs by not using the full amount of raw materials, not using any raw materials, or using raw materials illegally.

[0006] The technical solution adopted by the present invention to solve the above technical problems is as follows:

[0007] A method for detecting ginger in Chinese patent medicines based on high-resolution mass spectrometry technology, comprising the following steps:

[0008] S1. Collect representative ginger medicinal materials in multiple batches, extract them by water decoction respectively, and then dilute with an alcohol solvent to obtain the test solution of ginger water decoction. Weigh approximately 0.5 g of the simulated preparation of traditional Chinese medicine compound precisely, place it in a stoppered conical flask, accurately add 50 ml of 80% methanol, weigh it, ultrasonically treat for 30 minutes, let it cool, make up the weight with 80% methanol, shake well, filter, and take the continuous filtrate to obtain the test solution of the simulated preparation.

[0009] S2. Collect the total ion current chromatograms of each test solution under the conditions of ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry, compare with the complex traditional Chinese medicine compound system containing ginger water extract, and screen out the characteristic components, as shown in Figure 1 ;

[0010] S3. Identify the compound components according to the accurate mass numbers of the obtained characteristic components and the corresponding first-order and second-order mass spectrometry diagrams, and obtain the compound through literature and database search techniques.

[0011] S4. Optimize the mass spectrometry conditions in the multiple reaction monitoring (MRM) mode; establish a detection method according to the known characteristic components, the extraction conditions of the test samples, and the optimized chromatographic and mass spectrometry conditions.

[0012] S5. Use the method established in S4 above for the test samples to collect the characteristic compound reference substances and mass spectrometry diagrams of the test samples simultaneously. In the extracted ion current chromatogram of the test solution, the chromatographic peaks corresponding to the reference substances should be detected.

[0013] Preferably, in the above method, in S1, all the samples are identified as the fresh rhizomes of Zingiber officinale Rosc. of the Zingiberaceae family.

[0014] Preferably, in the above method, in S1, the alcohol reagent is 80% methanol (analytical grade); when extracting ginger, based on 50 g of Chinese medicinal materials, add 8 times the amount of water and decoct twice, each time for 2 hours; combine the decoctions, filter, concentrate to 50 ml, take 0.5 ml and dilute to 35 ml with 80% ethanol.

[0015] In the above method, in S1, the simulated preparation of traditional Chinese medicine compound includes the simulated preparation of traditional Chinese medicine compound containing ginger and the simulated preparation of traditional Chinese medicine compound without ginger; among them, the simulated preparation of traditional Chinese medicine compound containing ginger is prepared in the laboratory on a small scale according to the prescription amount and preparation method under the variety of Baoxinning Tablets; the difference between the simulated preparation of traditional Chinese medicine compound without ginger and the simulated preparation of traditional Chinese medicine compound containing ginger is that it does not contain ginger.

[0016] Preferably, in the above method, in S2, the ultra-high performance liquid chromatography uses the following conditions:

[0017] Chromatographic conditions: Chromatographic column: Agilent SB C18 (100 mm × 2.1 mm, 1.8 μm); Column temperature: 30 °C; Flow rate: 0.3 ml / min; Gradient elution was adopted, mobile phase A was acetonitrile, and mobile phase B was 0.1% formic acid aqueous solution; Based on the total volume of the mobile phase being 100%, in the 0 - 5 min, the volume of mobile phase A was 5%, and the volume of mobile phase B was 95%; In the 5 - 18 min, the volume of mobile phase A increased from 5% to 44%, and the volume of mobile phase B decreased from 95% to 56%.

[0018] Preferably, in the above method, in S2, the quadrupole time-of-flight mass spectrometry adopts the following conditions:

[0019] Ion source: Electrospray ionization (ESI); Positive ion scanning mode: Electrospray voltage: 5500 V; Ion source temperature: 550 °C; Curtain gas: 35 psi; Nebulizing gas: 55 psi; Auxiliary gas: 55 psi; Declustering voltage: 60 V; Collision voltage: 35 V; The scanning mode was full scan of the first-stage mass spectrometry and full scan of the second-stage mass spectrometry, and the scanning range was 100 - 1500 m / z; Reference ions m / z: 121.0480 and 922.0098.

[0020] Preferably, in the above method, in S3, according to the retention time, the first-stage accurate mass number and the second-stage mass spectrometry of the test sample, a library search and matching were carried out with the drug database in the mass spectrometry software to identify the characteristic compounds.

[0021] Preferably, in the above method, in S3, the screening process of the characteristic components was to collect MS / MS mass spectrometry data by UPLC-Q-TOF high-resolution mass spectrometry, import it into Agilent MPP software for PCA and multivariate discriminant analysis to screen the components with differences between groups; Combining with the verification of the reference quality spectrometry diagram, it was found that hexahydrocurcumin (the mass spectrometry information of the compound is shown in Table 1, and the typical mass spectrometry diagram is shown in Figure 2 ) is the characteristic component of ginger, with the CAS number of 36062 - 05 - 2; MS 1 (m / z) 375.1843 [M + H]+; MS 2 (m / z) 357.1736 [M + H]+, and a mass spectrometry determination method was established accordingly.

[0022] Table 1 Information table of hexahydrocurcumin compound

[0023]

[0024] Preferably, in the above method, in S4, the detection method is as follows: a chromatographic column (100 mm × 2.1 mm) filled with octadecylsilyl silica gel; column temperature: 30 °C; flow rate: 0.3 ml / min; using acetonitrile - 0.1% formic acid solution (25:75) as the mobile phase; in the multiple reaction monitoring (MRM) mode, select m / z357.2→177.1 and m / z357.2→145.0 as the detection ion pairs; in the extracted ion current chromatogram of the test sample, the chromatographic peak corresponding to the hexahydrocurcumin reference substance should be detected.

[0025] A method for detecting ginger in traditional Chinese patent medicine based on high-resolution mass spectrometry technology, comprising the following steps:

[0026] (1) Preparation of reference substance solution: Take an appropriate amount of the reference substance of the characteristic component hexahydrocurcumin, accurately weigh it, dissolve it with an alcohol reagent to obtain a reference substance solution;

[0027] (2) Preparation of test sample solution: Take the test sample, accurately weigh it, extract it with an alcohol reagent to obtain a test sample solution;

[0028] (3) Determination: Use ultra-high performance liquid chromatography combined with triple quadrupole mass spectrometry to collect the extracted ion current chromatograms of the reference substance solution and the test sample solution respectively; if a chromatographic peak corresponding to the hexahydrocurcumin reference substance is detected in the test sample, it indicates that the test sample contains ginger, otherwise it does not.

[0029] Preferably, in step (1), the screening method of the characteristic component comprises the following steps:

[0030] S1. Collect multiple batches of representative ginger medicinal materials, extract them by water decoction respectively, and then dilute them with an alcohol solvent to obtain a ginger water decoction test sample solution; Take about 0.5 g of the traditional Chinese medicine compound simulation preparation, accurately weigh it, place it in a stoppered conical flask, accurately add 50 ml of 80% methanol, weigh it, ultrasonically treat it for 30 minutes, let it cool, make up the weight with 80% methanol, shake well, filter, and take the subsequent filtrate to obtain the simulation preparation test sample solution;

[0031] S2. Use ultra-high performance liquid chromatography combined with quadrupole time-of-flight mass spectrometry conditions to collect the total ion current chromatograms of each test sample solution, compare them with the complex traditional Chinese medicine compound system containing ginger water extract, and screen out the characteristic components, as shown in Figure 1 ;

[0032] S3. According to the accurate mass number of the obtained characteristic component and the corresponding first-order and second-order mass spectrometry diagrams, identify the compound components through literature and database search technology, and obtain the compound.

[0033] Preferably, in step (1), the alcohol reagent is methanol; add the methanol to make a solution containing 0.5 μg per 1 ml to obtain the reference substance solution.

[0034] Preferably, in step (2), the alcohol reagent is 80% methanol; when extracting the test sample, 100 ml of 80% methanol is added, and ultrasonic treatment is carried out for 30 minutes.

[0035] Preferably, in step (2), the test sample is Baoxinning tablets; the Baoxinning tablets are ground finely, one tablet is weighed accurately, placed in a conical flask, 100 ml of 80% methanol is accurately added, weighed, ultrasonically treated for 30 minutes, cooled, the lost weight is made up with 80% methanol, shaken well, filtered, and the subsequent filtrate is taken to obtain the test sample solution.

[0036] Preferably, in step (2), the test sample is Baoxinning capsules; an appropriate amount of the content of the Baoxinning capsules under the difference in filling quantity is taken, ground finely, 0.3 g is taken, weighed accurately, placed in a conical flask, 100 ml of 80% methanol is accurately added, weighed, ultrasonically treated for 30 minutes, cooled, the lost weight is made up with 80% methanol, shaken well, filtered, and the subsequent filtrate is taken to obtain the test sample solution.

[0037] Preferably, it is characterized in that in step (3), 1 μl of each of the reference solution and the test sample solution is accurately pipetted and injected into a liquid chromatography - mass spectrometry instrument for determination.

[0038] Preferably, in step (3), the ultra - high performance liquid chromatography uses the following conditions:

[0039] A chromatographic column (100 mm × 2.1 mm) filled with octadecylsilyl silica gel; column temperature: 30 °C; flow rate: 0.3 ml / min; using acetonitrile - 0.1% formic acid solution (25:75) as the mobile phase.

[0040] Preferably, in step (3), the triple quadrupole mass spectrometry uses the following conditions:

[0041] Ion source: electrospray ionization (ESI); positive ion scan mode: electrospray voltage: 5500 V; ion source temperature: 550 °C; curtain gas: 35 psi; nebulizing gas: 55 psi; auxiliary gas: 55 psi; declustering voltage: 60 V; collision voltage: 35 V; multiple reaction monitoring (MRM) mode, selecting m / z357.2→177.1 and m / z357.2→145.0 as the detection ion pairs; reference ions m / z: 121.0480 and 922.0098.

[0042] Preferably, in step (3), in the reference solution, the signal - to - noise ratio of the MRM chromatographic peaks for ion pair determination is greater than 3:1.

[0043] Compared with the prior art, the beneficial effects of the present invention are:

[0044] (1) The present invention is mainly used for the detection of ginger in Chinese patent medicine. Chinese patent medicine is mostly made by extracting and processing Chinese medicine, and the appearance of the raw materials has been destroyed, making it difficult to determine whether the raw materials are added according to the prescription. The method uses high-resolution mass spectrometry technology to screen the specific component hexahydrocurcumin in the ginger water extract, and the detection thereof can quickly determine whether the Chinese patent medicine contains ginger.

[0045] (2) Ginger contains volatile oils and gingerols as main ingredients, but ginger is traditionally used in traditional Chinese medicines by decoction, which results in extremely low contents of these volatile and fat-soluble ingredients in traditional Chinese medicines, making them difficult to detect, thus bringing difficulties to drug quality inspection and supervision. Based on the above situation, the present invention screens for hexahydrocurcumin, a specific ingredient in ginger water extract, and develops a detection method based on ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry, which can effectively solve this problem in practical work.

[0046] (3) The key technical point of the present invention is that it adopts a method different from the method for detecting the main components of ginger, thereby improving the specificity and sensitivity of the method; on the other hand, the present invention finds a characteristic compound of ginger in the water extract of the traditional Chinese medicine compound, namely hexahydrocurcumin, which can be used to identify ginger, and can be detected quickly and effectively. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 This is a comparison of total ion currents of different ginger herbs;

[0048] Figure 2 This is a typical mass spectrum of Hexahydrocurcumin;

[0049] Figure 3 These are the mass spectrometry detection diagrams of the Baoxinning Chinese patent medicine preparation in Example 1 (A. MRM diagram of negative sample extraction, B. MRM diagram of reference substance extraction, C. MRM diagram of Baoxinning tablet sample extraction, D. MRM diagram of Baoxinning capsule sample extraction). DETAILED DESCRIPTION

[0050] In order to better understand the content of the present invention, further description is given below in conjunction with specific embodiments and accompanying drawings. It should be understood that these embodiments are only used to further illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content described in the present invention, those skilled in the art may make some non-essential changes or adjustments to the present invention, which still belong to the protection scope of the present invention.

[0051] Example 1

[0052] Study on ginger addition in Baoxinning Chinese patent medicine preparation:

[0053] 1.1 Chromatographic conditions

[0054] Chromatographic column: A chromatographic column packed with octadecylsilyl silica gel (100 mm × 2.1 mm), namely Agilent SB C18 (100 mm × 2.1 mm, 1.8 μm); Column temperature: 30 °C; Flow rate: 0.3 ml / min; Using acetonitrile - 0.1% formic acid solution (25:75) as the mobile phase.

[0055] 1.2 Mass spectrometry conditions

[0056] Ion source: Electrospray ionization (ESI); Positive ion scanning mode: Electrospray voltage: 5500 V; Ion source temperature: 550 °C; Curtain gas: 35 psi; Nebulizing gas: 55 psi; Auxiliary gas: 55 psi; Declustering voltage: 60 V; Collision voltage: 35 V; Multiple reaction monitoring (MRM) mode, select m / z 357.2 → 177.1 and m / z 357.2 → 145.0 as the detected ion pairs; Reference ions m / z: 121.0480 and 922.0098.

[0057] 1.3 Preparation of reference substance solution

[0058] Take an appropriate amount of hexahydrocurcumin reference substance, weigh accurately, dissolve in methanol to make a solution containing 0.5 μg per 1 ml, and you will get it.

[0059] 1.4 Preparation of test solution

[0060] (1) Tablets: Take 20 Baoxinning tablets, grind them finely, take about the weight of 1 tablet, weigh accurately, place in a conical flask, accurately add 100 ml of 80% methanol, weigh, ultrasonicate for 30 minutes, let it cool, make up the lost weight with 80% methanol, shake well, filter, and take the continuous filtrate, and you will get it.

[0061] (2) Capsules: Take an appropriate amount of the content of Baoxinning capsules under the difference in filling quantity, grind them finely, take about 0.3 g, weigh accurately, place in a conical flask, accurately add 100 ml of 80% methanol, weigh, ultrasonicate for 30 minutes, let it cool, make up the lost weight with 80% methanol, shake well, filter, and take the continuous filtrate, and you will get it.

[0062] 1.5 Determination method

[0063] Precisely pipette 1 μl of the reference substance solution and the test solution respectively, inject them into the liquid chromatography - mass spectrometry combined instrument for determination, and you will get it. In the reference substance solution, the signal - to - noise ratio of the MRM chromatographic peaks determined according to the above ion pairs should be greater than 3:1.

[0064] 1.6 Result determination

[0065] In the extracted ion current chromatogram of the test sample, the chromatographic peaks corresponding to the reference substance should be detected.

[0066] Figure 3Mass spectrometry detection chart of the Baoxinning Chinese patent medicine preparation in this embodiment (A. MRM extraction chart of negative sample (simulated preparation of traditional Chinese medicine compound without ginger), B. MRM extraction chart of reference substance, C. MRM extraction chart of Baoxinning tablet sample, D. MRM extraction chart of Baoxinning capsule sample); As can be seen from the figure, the target components in the ginger-containing compound preparation (i.e., Baoxinning tablets / capsules) can be successfully detected using this method.

[0067] The above description is not a limitation of the present invention, nor is the present invention limited to the above examples. Changes, modifications, additions, or substitutions made by those of ordinary skill in the art within the scope of the essence of the present invention shall also fall within the protection scope of the present invention.

Claims

1. A method for detecting ginger in traditional Chinese patent medicines based on high-resolution mass spectrometry technology, characterized in that, It includes the following steps: (1) Preparation of reference solution: Weigh an appropriate amount of the reference substance of the characteristic component hexahydrocurcumin precisely, dissolve it with an alcohol reagent to obtain a reference solution. (2) Preparation of test solution: Weigh the test sample precisely, extract it with an alcohol reagent to obtain a test solution. (3) Determination: Use ultra-high performance liquid chromatography combined with triple quadrupole mass spectrometry to collect the extracted ion current chromatograms of the reference solution and the test solution respectively; if a chromatographic peak corresponding to the hexahydrocurcumin reference substance is detected in the test sample, it indicates that the test sample contains ginger, otherwise it does not.

2. The method for detecting ginger in Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 1, wherein In step (1), the screening method of the characteristic component includes the following steps: S1. Collect representative ginger medicinal materials in multiple batches, extract them by water decoction respectively, and then dilute them with an alcohol solvent to obtain a test solution of ginger water decoction. Weigh approximately 0.5 g of the traditional Chinese medicine compound simulation preparation precisely, place it in a stoppered conical flask, precisely add 50 ml of 80% methanol, weigh it, ultrasonically treat it for 30 minutes, let it cool, make up the weight with 80% methanol, shake well, filter, and take the subsequent filtrate to obtain a test solution of the simulation preparation. S2. Use ultra-high performance liquid chromatography combined with quadrupole time-of-flight mass spectrometry conditions to collect the total ion current chromatograms of each test solution, compare them with the complex traditional Chinese medicine compound system containing ginger water extract, and screen out the characteristic components. S3. According to the accurate mass number of the obtained characteristic component and the corresponding first-order and second-order mass spectrometry diagrams, identify the compound components through literature and database search techniques, and obtain the compound.

3. The method for detecting ginger in Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 2, wherein, In step S1, the alcohol reagent is 80% methanol; when extracting ginger, based on 50 g of traditional Chinese medicine materials, add 8 times the amount of water and decoct for 2 times, 2 hours each time; combine the decoctions, filter, concentrate to 50 ml, take 0.5 ml and dilute it to 35 ml with 80% ethanol.

4. The method for detecting ginger in Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 2, wherein In step S2, the ultra-high performance liquid chromatography uses the following conditions: Chromatographic conditions: Chromatographic column: Agilent SB C18, 100 mm×2.1 mm, 1.8 μm; Column temperature: 30 °C; Flow rate: 0.3 ml / min; Gradient elution is adopted, mobile phase A is acetonitrile, and mobile phase B is 0.1% formic acid aqueous solution; Based on the total volume of the mobile phase being 100%, in the 0 - 5 min, the volume of mobile phase A is 5%, and the volume of mobile phase B is 95%; in the 5 - 18 min, the volume of mobile phase A increases from 5% to 44%, and the volume of mobile phase B decreases from 95% to 56%. The quadrupole time-of-flight mass spectrometry uses the following conditions: Ion source: Electrospray ionization; Positive ion scan mode: Electrospray voltage: 5500 V; Ion source temperature: 550 °C; Curtain gas: 35 psi; Nebulizing gas: 55 psi; Auxiliary gas: 55 psi; Declustering voltage: 60 V; Collision voltage: 35 V; The scanning mode is full scan of first-order mass spectrometry and full scan of second-order mass spectrometry, and the scanning range is 100 - 1500 m / z; Reference ions m / z: 121.0480 and 922.0098.

5. The method for detecting ginger in Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 2, wherein, In step S3, the screening process of the characteristic components is to collect MS / MS mass spectrometry data by UPLC-Q-TOF high-resolution mass spectrometry, import it into Agilent MPP software for PCA and multivariate discriminant analysis, and screen out the differential components between groups; combined with the verification of the control quality spectrum, hexahydrocurcumin is found to be the characteristic component of ginger, and a mass spectrometry determination method is established accordingly.

6. The method for detecting ginger in traditional Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 1, wherein, In step (1), the alcohol reagent is methanol; add the methanol to make a solution containing 0.5 μg per 1 ml, and the reference substance solution is obtained.

7. The method for detecting ginger in traditional Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 1, wherein, In step (2), the alcohol reagent is 80% methanol; when extracting the test sample, add 100 ml of 80% methanol and perform ultrasonic treatment for 30 minutes.

8. The method for detecting ginger in traditional Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 1, wherein, In step (2), the test sample is Baoxinning tablets; grind the Baoxinning tablets finely, weigh 1 tablet precisely, place it in a conical flask, precisely add 100 ml of 80% methanol, weigh, perform ultrasonic treatment for 30 minutes, cool, make up the lost weight with 80% methanol, shake well, filter, and take the subsequent filtrate to obtain the test sample solution. And / or the test sample is Baoxinning capsules; take an appropriate amount of the content of the Baoxinning capsules under the difference in filling quantity, grind it finely, take 0.3 g, weigh precisely, place it in a conical flask, precisely add 100 ml of 80% methanol, weigh, perform ultrasonic treatment for 30 minutes, cool, make up the lost weight with 80% methanol, shake well, filter, and take the subsequent filtrate to obtain the test sample solution.

9. The method for detecting ginger in traditional Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 1, wherein, In step (3), the ultra-high performance liquid chromatography adopts the following conditions: A chromatographic column filled with octadecylsilane-bonded silica gel, with a specification of 100 mm × 2.1 mm; column temperature: 30 °C; flow rate: 0.3 ml / min; using acetonitrile - 0.1% formic acid solution as the mobile phase, and the volume ratio of acetonitrile to 0.1% formic acid solution is 25:

75. The triple quadrupole mass spectrometry adopts the following conditions: Ion source: electrospray ionization; positive ion scan mode: electrospray voltage: 5500 V; ion source temperature: 550 °C; curtain gas: 35 psi; nebulizing gas: 55 psi; Auxiliary gas: 55 psi; declustering voltage: 60 V; collision voltage: 35 V; multiple reaction monitoring mode, select m / z357.2→177.1 and m / z357.2→145.0 as the detection ion pairs; reference ions m / z: 121.0480 and 922.0098.

10. The method for detecting ginger in traditional Chinese patent medicine based on high-resolution mass spectrometry technology according to claim 1, characterized in that, In step (3), in the reference substance solution, the signal-to-noise ratio of the MRM chromatographic peak for ion pair determination is greater than 3:1.

Images