Fingerprint detection method of red yeast rice

Abstract

The invention discloses a red yeast rice fingerprint spectrum detection method. The fingerprint detection method is developed for the monacolin compound in the monascus, whether the to-be-detected sample contains the monascus meeting the quality requirement or not can be directly judged by comparing the similarity of the to-be-detected sample and the contrast fingerprint, the detection efficiency is improved, and the detection cost is reduced.

Description

Technical Field

[0001] This invention relates to the field of analytical testing, and in particular to a fingerprint detection method for red yeast rice. Background Technology

[0002] Red yeast rice originated in my country and was anciently known as Danqu or red yeast rice. It is a dried rice grain produced by fermenting rice with Monascus spp. Since the 1970s, when Japanese scientist Akira Endo first isolated the lipid-lowering component monacolin K (lovastatin) from Monascus spp., and lovastatin was subsequently developed into a lipid-lowering drug, red yeast rice has been a hot topic in pharmaceutical research and has high economic value. However, identifying red yeast rice or components derived from red yeast rice added to traditional Chinese medicine or health products is time-consuming and laborious, making quality control of drugs or health products containing red yeast rice very difficult. Red yeast rice contains abundant secondary metabolites, making the development of fingerprint detection methods extremely difficult; currently, no fingerprint detection method for red yeast rice has been developed.

[0003] Monacolin-like compounds are the main source of the lipid-lowering activity of red yeast rice. Red yeast rice can produce various monacolin-like compounds, and the distribution of their content is directly related to its lipid-lowering effect. Developing a fingerprint-based detection method for monacolins in red yeast rice would not only aid in the identification and quality control of red yeast rice but also facilitate the comprehensive analysis and detection of monacolin-like compounds within it. Therefore, the development of a fingerprint-based detection method for red yeast rice is urgently needed in this field. Summary of the Invention

[0004] The purpose of this invention is to provide a fingerprint spectrum detection method for red yeast rice.

[0005] To address the aforementioned technical problems, a first aspect of the present invention provides a method for detecting the fingerprint spectrum of red yeast rice, the method comprising the steps of:

[0006] A fingerprint spectrum of the sample to be tested is obtained and compared with a control fingerprint spectrum. The similarity between the fingerprint spectrum of the sample to be tested and the control fingerprint spectrum is used to determine whether the sample to be tested contains red yeast rice. The control fingerprint spectrum is selected from... Figure 24 , Figure 25 and / or Figure 26 ;

[0007] The method for obtaining the fingerprint spectrum of the sample to be tested is as follows:

[0008] The sample to be tested is extracted using an extractant to obtain a test solution, wherein the extractant is a mixed solvent of acetonitrile and water with a volume ratio of 70:30; and

[0009] The test solution was analyzed using a liquid chromatography-tandem triple quadrupole mass spectrometer to obtain a fingerprint chromatogram of the sample. The chromatographic conditions of the liquid chromatography-tandem triple quadrupole mass spectrometer are as follows:

[0010] Column: Aglient Poroshell EC-C18 column;

[0011] Mobile phase: The organic phase is acetonitrile, and the aqueous phase is 0.1% formic acid solution as the mobile phase;

[0012] Elution method: gradient elution.

[0013] Injection volume: 1-5 μL;

[0014] The flow rate was 0.4 ml / min; and

[0015] The column temperature is 20℃;

[0016] The gradient elution procedure is as follows:

[0017] Time (minutes) Organic phase (%) Aqueous phase (%) 0～10 5→35 95→65 10～18 35 65 18～20 35→40 65→60 20～35 40→45 60→55 35～50 45→55 55→45 50～60 55→75 45→25 60～70 75→95 25→5 70～70.1 95→5 5→95

[0018] The mass spectrometry conditions for the liquid chromatography-tandem triple quadrupole mass spectrometry include: selecting a parent ion with a charge-to-mass ratio of 283.0 ± 1 and a daughter ion with a charge-to-mass ratio of 223.0 ± 1; and / or

[0019] Select a parent ion with a charge-to-mass ratio of 285.0 ± 1 and a daughter ion with a charge-to-mass ratio of 225.0 ± 1; and / or

[0020] A parent ion with a charge-to-mass ratio of 287.0±1 was selected, and a daughter ion with a charge-to-mass ratio of 227.0±1 was selected.

[0021] In some preferred embodiments, the method involves determining whether the fingerprint spectrum of the sample to be tested contains, for example, [the following]. Figure 24 , Figure 25 and / or Figure 26 The peaks shown are used to determine the similarity between the fingerprint spectrum of the sample to be tested and the control fingerprint spectrum.

[0022] In some preferred embodiments, when the peaks in the fingerprint spectrum of the sample to be tested are similar to... Figure 24 , Figure 25 and / or Figure 26 If the peaks in the top 80% (preferably 85%, more preferably 90%) of the mid-peak area values ​​are identical, then the sample to be tested or its preparation raw materials are considered to contain red yeast rice.

[0023] Figure 24 The retention times and peak areas of each peak are shown in Table A below:

[0024] Table A

[0025] serial number Retention time Peak area 1 5.426 1202 2 6.35 1747.185 3 7.019 8459.111 4 7.781 2165.741 5 7.943 7753.704 6 8.204 4982.037 7 9.197 2676.63 8 9.634 4060.63 9 9.807 1796.926 10 10.389 10850.04 11 10.934 25221.26 12 11.116 5039.111 13 11.482 2778.148 14 11.678 7681.371 15 11.843 2488.333 16 12.115 29261.74 17 12.45 8886.223 18 12.587 3076.778 19 12.875 3533.667 20 15.95 2184.259 21 17.46 6069.074 22 22.615 33118.262 23 35.961 9643.481 .

[0026] Figure 25 The retention times and peak areas of each peak are shown in Table B below:

[0027] Table B

[0028] serial number Retention time Peak area 1 16.302 6321.091 2 22.15 14172.24 3 24.127 3256.303 4 26.682 1894.667 5 28.057 3357.606 6 30.423 1709.667 7 31.429 5328.182 8 33.576 9684.818 9 36.704 2002.97 10 37.119 3169.121 11 41.759 151020.797 12 47.478 5267.667 13 49.771 1304.212 14 52.71 507793.094 15 62.153 42492.27 .

[0029] Figure 26 The retention times and peak areas of each peak are shown in Table C below:

[0030] Table C

[0031] serial number Retention time Peak area 1 14.389 3614.178 2 15.002 114533.602 3 21.055 140844.797 4 25.458 3896.643 5 34.336 15633.64 6 41.785 10831.07 7 42.51 5761.75 8 46.203 49913.109 9 50.926 58177.609 10 59.11 342989 11 66.453 46497.18 .

[0032] In some preferred embodiments, the similarity between the fingerprint spectrum of the sample to be tested and the control fingerprint spectrum is calculated using traditional Chinese medicine chromatography and fingerprint spectrum similarity evaluation software.

[0033] In some preferred embodiments, the sample to be tested or its preparation raw materials are considered to contain red yeast rice based on the similarity between the fingerprint spectrum of the sample to be tested and the control fingerprint spectrum being not less than 0.8 (preferably not less than 0.85; more preferably not less than 0.86; more preferably not less than 0.87; more preferably not less than 0.88; more preferably not less than 0.89; more preferably not less than 0.90).

[0034] In some preferred embodiments, when the mass spectrometry conditions of the liquid chromatography-tandem triple quadrupole mass spectrometry are: selecting a mother ion with a charge-to-mass ratio of 283.0±1 and a daughter ion with a charge-to-mass ratio of 223.0±1, the calculated fingerprint spectrum is compared with... Figure 24 The similarity is based on the fingerprint spectrum of the sample to be tested and Figure 24 The similarity is used to determine whether the sample to be tested or its preparation raw materials contain red yeast rice. Preferably, a parent ion with a charge-to-mass ratio of 283.0±1 and a daughter ion with a charge-to-mass ratio of 223.0±1 are selected. When the fingerprint spectrum of the sample to be tested and the... Figure 24 If the similarity is not less than 0.8 (preferably not less than 0.85; more preferably not less than 0.86; more preferably not less than 0.87; more preferably not less than 0.88; more preferably not less than 0.80; more preferably not less than 0.90), then the sample to be tested or its preparation raw materials are considered to contain red yeast rice.

[0035] In some preferred embodiments, when the mass spectrometry conditions of the liquid chromatography-tandem triple quadrupole mass spectrometry are: selecting a mother ion with a charge-to-mass ratio of 285.0±1 and a daughter ion with a charge-to-mass ratio of 225.0±1, the calculated fingerprint spectrum is compared with... Figure 25 The similarity between the fingerprint spectrum of the test sample and the control fingerprint spectrum is used to determine whether the test sample or its preparation raw materials contain red yeast rice. Preferably, a parent ion with a charge-to-mass ratio of 285.0±1 and a daughter ion with a charge-to-mass ratio of 225.0±1 are selected. Figure 25 If the similarity is not less than 0.8 (preferably not less than 0.85; more preferably not less than 0.86; more preferably not less than 0.87; more preferably not less than 0.88; more preferably not less than 0.80; more preferably not less than 0.90), then the sample to be tested or its preparation raw materials are considered to contain red yeast rice.

[0036] In some preferred embodiments, when the mass spectrometry conditions of the liquid chromatography-tandem triple quadrupole mass spectrometry are: selecting a mother ion with a charge-to-mass ratio of 287.0±1 and a daughter ion with a charge-to-mass ratio of 227.0±1, the calculated fingerprint spectrum is compared with... Figure 26 The similarity between the fingerprint spectrum of the test sample and the control fingerprint spectrum is used to determine whether the test sample or its preparation raw material contains red yeast rice. Preferably, a parent ion with a charge-to-mass ratio of 287.0±1 and a daughter ion with a charge-to-mass ratio of 227.0±1 are selected. Figure 26 If the similarity is not less than 0.8 (preferably not less than 0.85; more preferably not less than 0.86; more preferably not less than 0.87; more preferably not less than 0.88; more preferably not less than 0.80; more preferably not less than 0.90), then the sample to be tested or its preparation raw materials are considered to contain red yeast rice.

[0037] In some preferred schemes, a parent ion with a charge-to-mass ratio of 283.0 ± 1 and a daughter ion with a charge-to-mass ratio of 223.0 ± 1 are selected to obtain the first fingerprint spectrum of the sample to be tested; and

[0038] A precursor ion with a charge-to-mass ratio of 285.0 ± 1 and a daughter ion with a charge-to-mass ratio of 225.0 ± 1 were selected to obtain the second fingerprint spectrum of the sample to be tested; and

[0039] The parent ion with a charge-to-mass ratio of 287.0±1 and the daughter ion with a charge-to-mass ratio of 227.0±1 were selected to obtain the third fingerprint spectrum of the sample to be tested.

[0040] When the peaks in the first fingerprint spectrum of the sample to be tested are at least equal to Figure 24The peaks in the second fingerprint spectrum of the sample match the peaks in the top 80% (preferably 85%, more preferably 90%) of the mid-peak area, and the peaks in the second fingerprint spectrum of the sample match at least the peaks in the mid-peak area. Figure 25 The peaks in the middle peak area match the top 80% of the peaks, and the peaks in the second fingerprint spectrum of the sample being tested are at least... Figure 26 If the peaks in the middle peak area match the values ​​of the first 80% of the peaks, then the sample to be tested or its preparation raw materials are considered to contain red yeast rice.

[0041] When the first fingerprint spectrum of the sample to be tested is compared with the control fingerprint spectrum Figure 24 The similarity is not less than 0.8 (preferably not less than 0.85; more preferably not less than 0.86; more preferably not less than 0.87; more preferably not less than 0.88; more preferably not less than 0.89; more preferably not less than 0.90), and the second fingerprint spectrum of the sample to be tested is similar to the control fingerprint spectrum. Figure 25 The similarity is not less than 0.8 (preferably not less than 0.85; more preferably not less than 0.86; more preferably not less than 0.87; more preferably not less than 0.88; more preferably not less than 0.89; more preferably not less than 0.90); and the third fingerprint spectrum of the sample to be tested is similar to the control fingerprint spectrum. Figure 26 If the similarity is not less than 0.8 (preferably not less than 0.85; more preferably not less than 0.86; more preferably not less than 0.87; more preferably not less than 0.88; more preferably not less than 0.89; more preferably not less than 0.90), then the sample to be tested or its preparation raw materials are considered to contain red yeast rice.

[0042] In some preferred embodiments, the sample to be tested is traditional Chinese medicine or health product.

[0043] In some preferred embodiments, the collision energy of the liquid chromatography-tandem triple quadrupole mass spectrometer is 22-24 eV.

[0044] In some preferred embodiments, the declustering voltage of the liquid chromatography-tandem triple quadrupole mass spectrometer is 180-200V.

[0045] In some preferred embodiments, the mass spectrometry conditions for the liquid chromatography-tandem triple quadrupole mass spectrometry include:

[0046] With a clustering voltage of 180V and a collision capability of 24eV, a parent ion with a charge-to-mass ratio of 283.0±1 and a daughter ion with a charge-to-mass ratio of 223.0±1 are selected.

[0047] At a declustering voltage of 180V and a collisional capability of 24eV, a parent ion with a charge-to-mass ratio of 285.0±1 and a daughter ion with a charge-to-mass ratio of 225.0±1 are selected; and / or

[0048] With a declustering voltage of 200V and a collision capability of 22eV, a parent ion with a charge-to-mass ratio of 287.0±1 and a daughter ion with a charge-to-mass ratio of 227.0±1 are selected.

[0049] In some preferred embodiments, the mass spectrometry conditions for the liquid chromatography-tandem triple quadrupole mass spectrometry include:

[0050] Ion source: Electrospray, positive ion scanning mode ESI(+);

[0051] Monitoring method: MRM mode, ion source temperature 200~600℃ (preferably 450℃);

[0052] With a declustering voltage of 180V and a collision capability of 24eV, a parent ion with a charge-to-mass ratio of 283.0 and a daughter ion with a charge-to-mass ratio of 223.0 were selected.

[0053] At a declustering voltage of 180V and a collisional capability of 24eV, a parent ion with a charge-to-mass ratio of 285.0 and a daughter ion with a charge-to-mass ratio of 225.0 are selected; and / or

[0054] With a declustering voltage of 200V and a collision capability of 22eV, a parent ion with a charge-to-mass ratio of 287.0 and a daughter ion with a charge-to-mass ratio of 227.0 are selected.

[0055] In some preferred embodiments, the mass spectrometry conditions for the liquid chromatography-tandem triple quadrupole mass spectrometry further include:

[0056] Drying gas: 50-100 L / min (preferably 50 L / min);

[0057] Air curtain gas: 20-40 L / min (preferably 40 L / min);

[0058] Spray voltage 4500V.

[0059] Compared with the prior art, the present invention has at least the following advantages:

[0060] (1) The embodiments of the present invention have developed a fingerprint spectrum detection method for Monacolin compounds in red yeast rice. By comparing the similarity between the fingerprint spectrum of the sample to be tested and the control fingerprint spectrum, it can be directly determined whether the sample to be tested contains red yeast rice that meets the quality requirements, thereby improving detection efficiency and reducing detection costs.

[0061] (2) The fingerprint spectrum detection method for red yeast rice provided by the embodiments of the present invention can also be used to detect the high-value component Monaclin compound in red yeast rice.

[0062] It should be understood that, within the scope of this invention, the above-described technical features of this invention and the technical features specifically described below (such as in the embodiments) can be combined with each other to form new or preferred technical solutions. Due to space limitations, they will not be described in detail here. Attached Figure Description

[0063] One or more embodiments are illustrated by way of example with reference to the accompanying drawings, and these illustrative descriptions do not constitute a limitation on the embodiments.

[0064] Figure 1 It is an ion flow map of the 283.0→223.0 m / z channel;

[0065] Figure 2 It is an ion flow map of the 285.0→225.0 m / z channel;

[0066] Figure 3 It is an ion flow map of the m / z 287.0→227.0 channel;

[0067] Figure 4 It is an ion flow map of the m / z 289.0→229.0 channel;

[0068] Figure 5 It is the m / z 283.0→223.0 channel;

[0069] Figure 6 This is a magnified diagram of the peak assignments for the m / z 283.0→223.0 channel;

[0070] Figure 7 This is a magnified diagram of the peak assignments for the m / z 283.0→223.0 channel;

[0071] Figure 8 It is the m / z 285.0→225.0 channel;

[0072] Figure 9 This is a magnified diagram of the peak assignments for the m / z 285.0→225.0 channel;

[0073] Figure 10 This is a magnified diagram of the peak assignments for the m / z 285.0→225.0 channel;

[0074] Figure 11 This is a magnified diagram of the peak assignments for the m / z 285.0→225.0 channel;

[0075] Figure 12 This is a magnified diagram of the peak assignments for the m / z 285.0→225.0 channel - 4;

[0076] Figure 13 It is the m / z 287.0→227.0 channel;

[0077] Figure 14 This is a magnified diagram of the peak assignments for the m / z 287.0→227.0 channel - 1;

[0078] Figure 15 This is a magnified diagram of the peak assignments for the m / z 287.0→227.0 channel;

[0079] Figure 16 This is a magnified diagram of the peak assignments for the m / z 287.0→227.0 channel - 3;

[0080] Figure 17 It is the m / z 287.0→227.0 channel;

[0081] Figure 18 It is an ion flow map of the 285.0→225.0 m / z channel;

[0082] Figure 19 It is an ion flow map of the m / z 285.0→239.0 channel;

[0083] Figure 20 It is an ion flow map of the 285.0→267.0 m / z channel;

[0084] Figure 21 It is an ion flow map of the m / z 285.0→199.0 channel;

[0085] Figure 22 It is an ion flow map of the m / z 285.0→169.0 channel;

[0086] Figure 23 It is an ion flow map of the 285.0→155.0 m / z channel;

[0087] Figure 24The fingerprint spectrum of the m / z 283.0→223.0 channel shows the following peaks: 1: Unknown-1; 2: Unknown-2; 3: Unknown-3; 4: Unknown-4; 5: Unknown-5; 6: 3,5-dihydroxy-3,5-dihydromonacolin J; 7: Unknown-6; 8: 3,5-dihydroxy-3,5-dihydrodehydromonacolin J; 9: Unknown-7; 10: Unknown-8; 11: Monacolin S acid; 12: Unknown-9; 13: Unknown-10; 14: Unknown-11; 15: Unknown-12; 16: Monacolin S; 17: Dehydromonacolin S acid; 18: Unknown-13; 19: Unknown-14; 20: 13-8-(2”-methyl butanoyloxy)monacophenyl; 21: α,β-hydromonacolin Q acid; 22: Monacolin Q. Acid peak 23: α,β-hydromonacolin Q;

[0088] Figure 25 The fingerprint spectrum of the m / z 285.0→225.0 channel shows the following peaks: 1: Monacolin J acid; 2: Monacolin J; 3: 3-hydroxy-3,5-dihydromonacolin K; 4: Dihydromonacolin J; 5: Monacolin M; 6: Monacolin X acid and Dehydromonacolin M acid; 7: 3”-hydroxydehydromonacolin Kacid; 8: Monacolin NT2; 9: Monacolin N; 10: Dehydromonacolin X acid; 11: Monacolin X; 12: Monacolin NT1 and Monacolin K acid; 13: Unkwon-1; 14: 3”-hydroxydehydromonacolin K and Dehydromonacolin N; 15: Monacolin K; 16: Dehydromonacolin K.

[0089] Figure 26The fingerprint spectrum of the m / z 287.0→227.0 channel shows the following peaks: Peak 1: Monacolin R acid; Peak 2: 3-hydroxy-3,5-dihydromonacolin L acid; Peak 3: Monacolin R acid; Peak 4: Dihydromonacolin J acid; Peak 5: Monacolin L acid; Peak 6: Dihydromonacolin N acid; Peak 7: Monacolin L acid; Peak 8: Dehydromonacolin L acid and Dihydromonacolin K acid; Peak 9: Dihydromonacolin K acid; Peak 10: Dehydrodihydromonacolin K acid.

[0090] Figure 27 This is a superimposed fingerprint spectrum of Monacolin-like compounds with a key ion mass number m / z of 283 in red yeast rice;

[0091] Figure 28 This is a superimposed fingerprint spectrum of Monacolin-like compounds with a key ion mass number m / z of 285 in red yeast rice;

[0092] Figure 29 This is a superimposed fingerprint spectrum of Monacolin-like compounds with a key ion mass number m / z of 287 in red yeast rice.

[0093] Figure 30 It is a superimposed fingerprint spectrum of monacolin-like compounds with a key ion mass number m / z of 283 in traditional Chinese medicine preparations containing red yeast rice;

[0094] Figure 31 It is a superimposed fingerprint spectrum of monacolin-like compounds with a key ion mass number m / z of 285 in traditional Chinese medicine preparations containing red yeast rice;

[0095] Figure 32 This is a superimposed fingerprint spectrum of monacolin-like compounds with a key ion mass number m / z of 287 in traditional Chinese medicine preparations containing red yeast rice. Detailed Implementation

[0096] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the present invention is further described below in conjunction with specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Experimental methods in the following embodiments that do not specify specific conditions are generally performed under conventional conditions or as recommended by the manufacturer. Unless otherwise stated, percentages and parts are weight percentages and parts by weight. Unless otherwise specified, the experimental materials and reagents used in the following embodiments are commercially available.

[0097] Unless otherwise specified, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains. It should be noted that the terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the exemplary embodiments of this application.

[0098] Unless otherwise specified, the term “or” means the term “and / or” and is used interchangeably with the term “and / or”.

[0099] As used herein, including the appended claims, unless the context clearly indicates otherwise, the singular forms of words such as “an,” “a,” and “the” include their respective plural referents.

[0100] Example 1: Pretreatment Method

[0101] Take approximately 0.5 g of the test sample powder (passed through a No. 3 sieve), accurately weigh it, and place it in a stoppered conical flask. Accurately add 50 mL of acetonitrile-water (volume ratio 70:30) mixed solution, weigh it, sonicate for 30 minutes, cool it, replenish the lost weight with acetonitrile-water (volume ratio 70:30) mixed solution, centrifuge for 5 minutes (centrifugation speed 4000 r / min), take the supernatant, filter it through a microporous membrane (0.22 μm), and take the filtrate.

[0102] Example 2: Chromatographic and Mass Spectrometric Conditions

[0103] (1) Chromatographic conditions

[0104] An Agilent 1290 ultra-high performance liquid chromatograph was used, with an Agilent Poroshell EC-C18 column (150 mm length, 3.0 mm inner diameter, 2.7 μm particle size). Acetonitrile was used as mobile phase A, and 0.1% formic acid solution was used as mobile phase B, with gradient elution performed according to the specifications in Table 2-1. The flow rate was 0.4 mL / min, and the column temperature was 20 °C. Injection volume: 0.1–5 μL.

[0105] Table 2-1 Elution gradient of mobile phase

[0106] Time (minutes) Mobile phase A (%) Mobile phase B (%) 0～10 5→35 95→65 10～18 35 65 18～20 35→40 65→60 20～35 40→45 60→55 35～50 45→55 55→45 50～60 55→75 45→25 60～70 75→95 25→5 70～70.1 95→5 5→95

[0107] (2) Mass spectrometry conditions: triple quadrupole tandem mass spectrometry

[0108] The AB5500 triple quadrupole tandem mass spectrometer uses an electrospray ionization (ESI) system in positive ion scanning mode (ESI+). Monitoring mode is MRM mode, with an ion source temperature of 450℃. Drying gas flow rate is 50 L / min, curtain gas flow rate is 40 L / min, and spray voltage is 4500 V. The mass spectrometry parameters for the four key component ions are shown in Table 2-2 below.

[0109] Table 2-2 Key Faction Ion Mass Spectrometry Parameters

[0110]

[0111]

[0112] The collected red yeast rice samples were analyzed using a triple quadrupole method, and ion chromatograms of each channel were extracted. Figure 1-4 The chromatographic peaks in the sample were assigned based on the material basis results, and the results are as follows: Figure 5-17 As shown, this method can effectively filter out interference from other compounds, specifically reveal the distribution of monacolin-like compounds, and can screen for and discover new monacolin-like compounds.

[0113] Example 3: Key Faction Ion Analysis

[0114] Since triple quadrupole mass spectrometry has lower qualitative capabilities than high-resolution mass spectrometry, the MRM mode is used for triple quadrupole mass spectrometry. The key daughter ion of the monocorine-like compound is used as the parent ion, and the daughter ion of the key daughter ion is used as the daughter ion. This allows us to obtain the distribution of the key daughter ion specific to the monocorine-like compound, and thus obtain the distribution of the monocorine-like compound.

[0115] The mass number m / z assigned to monacolin K (lovastatin) and monacolin acid is 285 (C). 19 H 25 O2 + Taking the key daughter ion as the parent ion as an example, using it as the parent ion, daughter ions with mass numbers m / z of 225, 267, 239, 199, 169, and 155 were obtained through daughter ion scanning. These seven daughter ions, ordered by response, are 225, 199, 267, 169, 239, and 155. According to... Figures 5-17 It can be seen that the mass spectral peaks in the obtained spectrum can indicate the presence of monacolin-like compounds at that retention time, and a high daughter ion mass spectral response can uncover more monacolin-like compounds. Therefore, from the perspective of daughter ion response, the 225 daughter ion is selected.

[0116] Simultaneous comparison of the ion chromatograms of each daughter ion channel reveals that the relative response of the mass spectrum peaks in the ion chromatogram of daughter ion 225 is closest to that in the extracted ion chromatogram of monacolin-like compounds in high-resolution mass spectrometry. In contrast, the relative responses of the mass spectrum peaks in the ion chromatogram of daughter ion 199 differ significantly from the responses of other mass spectrum peaks. Among them, the Dehydromonacolin K at 62.2 minutes has the highest response, rather than the highest response of the most abundant monacolin K and acid monacolin K.

[0117] In summary, considering the high response of each daughter ion and the relatively high similarity to the responses of the parent ions of various monacolin-like compounds in high-resolution mass spectrometry, 225 was selected as the exclusive daughter ion of the key daughter ion with a mass number m / z of 285.

[0118] Example 4

[0119] Based on the method in this patent, a fingerprinting method for monacolin-like compounds in red yeast rice was established using liquid chromatography-tandem triple quadrupole mass spectrometry. Specific non-targeted detection of monacolin-like compounds was performed on 28 batches of collected samples. 48 common peaks from the 28 batches were counted, and the fingerprinting of monacolin-like compounds in red yeast rice was generated by combining the specific spectra of the monacolin-like samples from the 28 batches. The details are as follows:

[0120] For monacolin-like compounds with a key ion mass number m / z of 283, 23 common peaks were identified. The area of ​​these 23 common peaks exceeds 85% of the total peak area and can comprehensively represent this type of monacolin-like compound. A fingerprint spectrum of this type of monacolin-like compound was established based on these 23 common peaks.

[0121] For monacolin-like compounds with a key ion mass number m / z of 285, 15 common peaks were identified. The area of ​​these 15 common peaks exceeds 85% of the total peak area, which can comprehensively represent this type of monacolin-like compound. A fingerprint spectrum of this type of monacolin-like compound was established based on these 15 common peaks.

[0122] For monacolin-like compounds with a key ion mass number m / z of 287, 10 common peaks were identified. The area of ​​these 10 common peaks exceeds 85% of the total peak area, which can comprehensively represent this type of monacolin-like compound. A fingerprint spectrum of this type of monacolin-like compound was established based on these 10 common peaks.

[0123] For monacolin-like compounds with a key ion mass number m / z of 289, fingerprinting was not established for this class of monacolin-like compounds due to their small number and low response.

[0124] The chromatographic conditions, mass spectrometry conditions, and preparation of the test solution are the same as above.

[0125] Preparation of reference solution: Weigh an appropriate amount of lovastatin reference standard accurately, add 70% acetonitrile to prepare a solution containing 1 μg per 1 ml.

[0126] Determination method: ① Accurately pipette 1-5 μl each of the reference solution and the test solution, inject them into the liquid chromatograph, and determine the fingerprint chromatograms of monacolin-like compounds with key ion mass numbers m / z of 287 and 283, respectively. ② Accurately pipette 0.2-1 μl each of the reference solution and the test solution, inject them into the liquid chromatograph, and determine the fingerprint chromatograms of monacolin-like compounds with key ion mass numbers m / z of 285.

[0127] In a fingerprint chromatogram with a key ion mass number m / z of 283, the test sample chromatogram should exhibit 23 characteristic peaks. The similarity between the test sample's characteristic chromatogram and the reference characteristic chromatogram was calculated using the Traditional Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System (version 2.0) based on the Mark peaks.

[0128] In a fingerprint chromatogram with a key ion mass number m / z of 285, the test sample chromatogram should exhibit 15 characteristic peaks, of which peak 14 should correspond to the retention time of the reference peak. A similarity evaluation system for chromatographic fingerprints of traditional Chinese medicine was used to calculate the similarity between the characteristic chromatograms of the test sample and the reference chromatogram based on the Mark peak.

[0129] In a fingerprint chromatogram with a key ion mass number m / z of 287, the test sample chromatogram should exhibit 10 characteristic peaks. A similarity evaluation system for chromatographic fingerprints of traditional Chinese medicine was used to calculate the similarity between the characteristic chromatogram of the test sample and the control chromatogram based on the Mark peak.

[0130] (1) Parallelism test of reference solution

[0131] Accurately pipette 1 μl of the reference solution and inject it 6 times consecutively. Record the peak area and calculate the RSD value. The results are shown in Table 4-1 below.

[0132] Table 4-1 Precision Test

[0133] lovastatin f1 2.05E+05 f2 2.04E+05 f3 2.07E+05 f4 2.01E+05 f5 2.02E+05 f6 2.06E+05 average 2.04E+05 RSD 1.1％

[0134] (2) Stability test of the test solution

[0135] Samples were taken and test solutions were prepared according to the prescribed method. The solutions were injected and analyzed at 0, 6, 12, 18, and 24 hours. The results showed that the retention times and peak areas of each compound in the test solutions were basically stable within 0–24 hours (see Tables 4-2 to 4-10).

[0136] Table 4-2 Stability tests (similarity) of Monacolin-like compounds with a key daughter ion mass number m / z of 283.

[0137] time Y1 0h 0.987 6h 0.986 12h 0.981 18h 0.985 24h 0.985 average 0.985 RSD% 0.2

[0138] Table 4-3 Stability tests (retention time / min) of Monacolin-like compounds with a key daughter ion mass number m / z of 283.

[0139] time Peak 1 Peak 2 Peak 3 Peak 4 Peak 5 Peak 6 Peak 7 Peak 8 Peak 9 Peak 10 Peak 11 0h 5.45 6.38 7.03 7.81 7.97 8.22 9.22 9.66 9.82 10.42 10.96 6h 5.45 6.38 7.03 7.8 7.97 8.23 9.22 9.67 9.83 10.43 10.97 12h 5.45 6.39 7.04 7.8 7.97 8.22 9.22 9.67 9.83 10.43 10.97 18h 5.44 6.37 7.03 7.8 7.97 8.23 9.21 9.66 9.82 10.42 10.96 24h 5.44 6.38 7.03 7.8 7.96 8.22 9.21 9.66 9.82 10.42 10.97 average 5.45 6.38 7.03 7.80 7.97 8.22 9.22 9.66 9.82 10.42 10.97 RSD% 0.1 0.1 0 0 0 0 0 0 0 0 0 time Peak 12 Peak 13 Peak 14 Peak 15 Peak 16 Peak 17 Peak 18 Peak 19 Peak 20 Peak 21 Peak 22 0h 11.13 11.5 11.69 11.85 12.13 12.46 12.59 12.89 16.11 17.51 22.8 6h 11.14 11.51 11.7 11.86 12.14 12.47 12.6 12.9 16.13 17.53 22.83 12h 11.13 11.51 11.7 11.86 12.14 12.47 12.6 12.9 16.12 17.55 22.83 18h 11.12 11.5 11.69 11.85 12.13 12.47 12.59 12.89 16.11 17.51 22.8 24h 11.13 11.51 11.69 11.85 12.13 12.47 12.6 12.89 16.11 17.51 22.8 average 11.13 11.51 11.69 11.85 12.13 12.47 12.60 12.89 16.12 17.52 22.81 RSD% 0 0 0 0 0 0 0 0 0 0.1 0

[0140] Table 4-4 Stability tests (peak areas) of monacolin-like compounds with a key daughter ion mass number m / z of 283.

[0141]

[0142]

[0143] Table 4-5 Stability tests (similarity) of Monacolin-like compounds with a key daughter ion mass number m / z of 285.

[0144] time Y1 0h 1 6h 1 12h 1 18h 1 24h 1 average 1 RSD% 0

[0145] Table 4-6 Stability tests (retention time / min) of monacolin-like compounds with a key daughter ion mass number m / z of 285.

[0146]

[0147]

[0148] Table 4-7 Stability tests (peak areas) for monacolin-like compounds with a key daughter ion mass number m / z of 285.

[0149] time Peak 1 Peak 2 Peak 3 Peak 4 Peak 5 Peak 6 Peak 7 Peak 8 0h 1.65E+06 5.47E+06 1.13E+06 1.04E+06 3.67E+05 1.04E+06 4.57E+05 2.35E+06 6h 1.51E+06 5.50E+06 1.11E+06 1.02E+06 3.70E+05 1.08E+06 4.86E+05 2.32E+06 12h 1.58E+06 5.13E+06 1.09E+06 1.02E+06 3.48E+05 1.05E+06 4.85E+05 2.24E+06 18h 1.55E+06 5.12E+06 1.07E+06 9.94E+05 3.52E+05 1.06E+06 4.76E+05 2.20E+06 24h 1.50E+06 5.12E+06 1.10E+06 9.95E+05 3.48E+05 1.02E+06 4.73E+05 2.16E+06 average 1.56E+06 5.27E+06 1.10E+06 1.01E+06 3.57E+05 1.05E+06 4.75E+05 2.25E+06 RSD% 3.8 3.7 2.0 1.9 3.0 2.1 2.4 3.5 time Peak 9 Peak 10 Peak 11 Peak 12 Peak 13 Peak 14 Peak 15 Peak 16 0h 2.78E+06 1.17E+06 1.16E+06 5.22E+07 1.72E+06 6.53E+05 1.30E+08 7.74E+06 6h 2.71E+06 1.20E+06 1.17E+06 5.22E+07 1.70E+06 6.35E+05 1.29E+08 8.41E+06 12h 2.69E+06 1.20E+06 1.15E+06 5.08E+07 1.59E+06 6.35E+05 1.28E+08 8.38E+06 18h 2.59E+06 1.21E+06 1.01E+06 5.08E+07 1.68E+06 6.78E+05 1.30E+08 8.32E+06 24h 2.57E+06 1.14E+06 1.03E+06 4.98E+07 1.52E+06 6.20E+05 1.28E+08 8.19E+06 average 2.67E+06 1.18E+06 1.10E+06 5.11E+07 1.64E+06 6.44E+05 1.29E+08 8.21E+06 RSD% 3.3 2.6 6.8 2.0 5.0 3.4 0.8 3.3

[0150] Table 4-8 Stability tests (similarity) of Monacolin-like compounds with a key daughter ion mass number m / z of 287.

[0151] time Y1 0h 0.999 6h 0.999 12h 0.997 18h 0.997 24h 0.999 average 0.9 RSD% 0.1

[0152] Table 4-9 Stability tests (retention time / min) of Monacolin-like compounds with a key daughter ion mass number m / z of 287.

[0153] time Peak 1 Peak 2 Peak 3 Peak 4 Peak 5 Peak 6 Peak 7 Peak 8 Peak 9 Peak 10 0h 14.39 15 21.05 25.45 34.31 42.48 46.18 50.89 59.09 66.45 6h 14.41 15.02 21.08 25.48 34.36 42.52 46.22 50.94 59.12 66.45 12h 14.41 15.03 21.09 25.49 34.36 42.52 46.22 50.94 59.12 66.46 18h 14.38 15.00 21.05 25.45 34.30 42.48 46.17 50.89 59.1 66.45 24h 14.39 15.01 21.05 25.46 34.31 42.48 46.17 50.9 59.1 66.44 average 14.40 15.01 21.06 25.47 34.33 42.50 46.19 50.91 59.11 66.45 RSD% 0 0 0 0 0 0 0 0 0 0

[0154] Table 4-10 Stability tests (peak areas) for monacolin-like compounds with a key daughter ion mass number m / z of 287.

[0155]

[0156]

[0157] (3) Repeatability test

[0158] Take six samples, prepare six test solutions according to the proposed method, and inject them for determination. The results are shown in Table 4-11 below. The results indicate that the method has good repeatability.

[0159] Table 4-11 Repeatability tests (similarity) of Monacolin-like compounds with a key ion mass number m / z of 283.

[0160] Self-numbered Peak 1 Sample 1-1 0.986 Sample 1-2 0.988 Sample 1-3 0.987 Samples 1-4 0.986 Samples 1-5 0.986 Samples 1-6 0.985 average 1.0 RSD% 0.1

[0161] Table 4-12 Repeatability tests (retention time / min) for Monacolin-like compounds with a key daughter ion mass number m / z of 283.

[0162] Self-numbered Peak 1 Peak 2 Peak 3 Peak 4 Peak 5 Peak 6 Peak 7 Peak 8 Peak 9 Peak 10 Peak 11 Sample 1-1 5.34 6.3 6.97 7.76 7.93 8.19 9.2 9.65 9.81 10.41 10.95 Sample 1-2 5.45 6.38 7.03 7.8 7.97 8.23 9.21 9.67 9.83 10.43 10.97 Sample 1-3 5.45 6.39 7.04 7.8 7.97 8.22 9.22 9.67 9.83 10.43 10.97 Samples 1-4 5.41 6.36 7.02 7.8 7.96 8.22 9.2 9.64 9.8 10.4 10.94 Samples 1-5 5.44 6.38 7.03 7.8 7.96 8.22 9.21 9.66 9.83 10.43 10.97 Samples 1-6 5.45 6.39 7.03 7.8 7.97 8.23 9.22 9.67 9.83 10.43 10.97 average 5.42 6.37 7.02 7.79 7.96 8.22 9.21 9.66 9.82 10.42 10.96 RSD% 0.8 0.5 0.3 0.2 0.1 0.1 0 0.1 0.1 0.1 0.1 Self-numbered Peak 12 Peak 13 Peak 14 Peak 15 Peak 16 Peak 17 Peak 18 Peak 19 Peak 20 Peak 21 Peak 22 Sample 1-1 11.12 11.5 11.68 11.85 12.13 12.46 12.59 12.88 16.1 17.51 22.8 Sample 1-2 11.13 11.5 11.69 11.85 12.13 12.47 12.6 12.89 16.11 17.52 22.82 Sample 1-3 11.14 11.51 11.7 11.86 12.14 12.47 12.6 12.9 16.11 17.53 22.82 Samples 1-4 11.11 11.49 11.68 11.84 12.12 12.45 12.58 12.87 16.07 17.47 22.78 Samples 1-5 11.13 11.5 11.69 11.86 12.14 12.47 12.6 12.9 16.12 17.53 22.83 Samples 1-6 11.13 11.51 11.7 11.86 12.14 12.47 12.6 12.89 16.12 17.52 22.81 average 11.13 11.50 11.69 11.85 12.13 12.47 12.60 12.89 16.11 17.51 22.81 RSD% 0 0 0 0 0 0 0 0 0.1 0.1 0

[0163] Table 4-13 Repeatability tests (peak areas) for Monacolin-like compounds with a key daughter ion mass number m / z of 283.

[0164]

[0165] Table 4-14 Repeatability tests (similarity) of Monacolin-like compounds with a key ion mass number m / z of 285.

[0166] Self-numbered Peak 1 Sample 1-1 1.000 Sample 1-2 0.979 Sample 1-3 1.000 Samples 1-4 1.000 Samples 1-5 1.000 Samples 1-6 1.000 average 1.000 RSD% 0.8

[0167] Table 4-15 Repeatability tests (retention time / min) for Monacolin-like compounds with a key ion mass number m / z of 285.

[0168]

[0169]

[0170] Table 4-16 Repeatability tests (peak areas) for Monacolin-like compounds with a key daughter ion mass number m / z of 285.

[0171]

[0172] Table 4-17 Repeatability tests (similarity) of Monacolin-like compounds with a key daughter ion mass number m / z of 287.

[0173] Self-numbered Peak 1 Sample 1-1 0.999 Sample 1-2 0.998 Sample 1-3 0.999 Samples 1-4 1.000 Samples 1-5 0.999 Samples 1-6 1.000 average 1.000 RSD% 0.0

[0174] Table 4-18 Repeatability tests (retention time / min) for Monacolin-like compounds with a key ion mass number m / z of 287.

[0175]

[0176]

[0177] Table 4-19 Repeatability tests (peak areas) for Monacolin-like compounds with a key ion mass number m / z of 287.

[0178] Self-numbered Peak 1 Peak 2 Peak 3 Peak 4 Peak 5 Sample 1-1 3.56E+05 8.55E+06 1.63E+07 5.34E+05 1.57E+06 Sample 1-2 3.48E+05 8.02E+06 1.52E+07 4.93E+05 1.58E+06 Sample 11-3 3.48E+05 8.50E+06 1.50E+07 5.17E+05 1.58E+06 Samples 1-4 3.19E+05 8.56E+06 1.48E+07 4.90E+05 1.64E+06 Samples 1-5 3.37E+05 8.10E+06 1.49E+07 4.91E+05 1.61E+06 Samples 1-6 3.17E+05 8.45E+06 1.49E+07 5.09E+05 1.64E+06 average 3.37E+05 8.36E+06 1.52E+07 5.06E+05 1.60E+06 RSD% 4.8 2.8 3.7 3.5 1.9 Self-numbered Peak 6 Peak 7 Peak 8 Peak 9 Peak 10 Sample 1-1 5.68E+05 4.72E+06 4.88E+06 3.02E+07 6.88E+06 Sample 1-2 5.80E+05 4.64E+06 4.85E+06 2.99E+07 6.04E+06 Sample 1-3 5.69E+05 4.71E+06 4.75E+06 2.89E+07 5.95E+06 Samples 1-4 5.60E+05 4.70E+06 4.74E+06 2.84E+07 5.66E+06 Samples 1-5 5.66E+05 4.61E+06 4.71E+06 2.85E+07 5.57E+06 Samples 1-6 5.60E+05 4.48E+06 4.69E+06 2.78E+07 5.43E+06 average 5.67E+05 4.64E+06 4.77E+06 2.90E+07 5.92E+06 RSD% 1.3 1.9 1.6 3.2 8.8

[0179] (4) Sample determination

[0180] Following the proposed method, 28 batches of samples were analyzed, and the results are shown in Table 4-20 below. The similarity was calculated by comparing the fingerprint spectra of the 28 batches of samples with those of the control sample. The fingerprint spectra of monacolin-like compounds with a key ion mass number (m / z) of 283 in 25 batches of samples showed a similarity greater than 0.90; the fingerprint spectra of monacolin-like compounds with a key ion mass number (m / z) of 285 in 27 batches of samples showed a similarity greater than 0.90; and the fingerprint spectra of monacolin-like compounds with a key ion mass number (m / z) of 287 in 25 batches of samples showed a similarity greater than 0.90. This is the first comprehensive analysis of the distribution and relative content of monacolin-like compounds in red yeast rice, indicating that the types and content distribution of monacolin-like compounds in red yeast rice are consistent.

[0181] Table 4-20 Sample Similarity Measurement Results

[0182]

[0183]

[0184] Example 5

[0185] In this embodiment, the traditional Chinese medicine preparations containing red yeast rice, namely, Lipitor Tablets and Xuezhikang Capsules, were tested according to the proposed method. The results showed that the chromatograms of both preparations contained the 48 chromatographic peaks specified in the method. The similarity results between these peaks and the fingerprint chromatograms generated from 28 batches of red yeast rice samples are shown in Table 5-1 below, indicating that this method can be used to test traditional Chinese medicine preparations containing red yeast rice. However, the similarity between the two preparations and the 28 batches of red yeast rice is relatively small. Therefore, the method described in this invention can be used to establish corresponding reference fingerprint chromatograms based on the distribution of monacolin compounds in different red yeast rice products, and then conduct similarity detection to comprehensively control the distribution and content of monacolin compounds in red yeast rice products.

[0186] Table 5-1 Results of similarity determination of traditional Chinese medicine preparations containing red yeast rice

[0187]

[0188] Those skilled in the art will understand that the above embodiments are specific examples of implementing the present invention, and in practical applications, various changes in form and detail may be made without departing from the spirit and scope of the present invention.

Claims

1. A method for detecting the fingerprint spectrum of red yeast rice, characterized in that, The method includes the following steps: Obtain the fingerprint spectrum of the sample to be tested and compare it with the control fingerprint spectrum. Determine whether the sample to be tested contains red yeast rice based on the similarity between the fingerprint spectrum of the sample to be tested and the control fingerprint spectrum. The control fingerprint spectrum is selected from Figure 24, Figure 25 and / or Figure 26. The method for obtaining the fingerprint spectrum of the sample to be tested is as follows: The sample to be tested was extracted using an extractant to obtain a test solution, wherein the extractant was a mixed solvent of acetonitrile and water with a volume ratio of 70:30; and The test solution was analyzed using a liquid chromatography-tandem triple quadrupole mass spectrometer to obtain a fingerprint chromatogram of the sample. The chromatographic conditions of the liquid chromatography-tandem triple quadrupole mass spectrometer are as follows: Column: Aglient Poroshell EC-C18 column; Mobile phase: The organic phase is acetonitrile, and the aqueous phase is 0.1% formic acid solution as the mobile phase; Elution method: gradient elution. Injection volume: 1-5 μL; The flow rate was 0.4 ml / min; and The column temperature is 20℃; The gradient elution procedure is as follows: The mass spectrometry conditions for the liquid chromatography-tandem triple quadrupole mass spectrometry include: selecting a parent ion with a charge-to-mass ratio of 283.0 ± 1 and a daughter ion with a charge-to-mass ratio of 223.0 ± 1; and / or Select a parent ion with a charge-to-mass ratio of 285.0 ± 1 and a daughter ion with a charge-to-mass ratio of 225.0 ± 1; and / or Select a parent ion with a charge-to-mass ratio of 287.0±1 and a daughter ion with a charge-to-mass ratio of 227.0±1; Preferably, the similarity between the fingerprint spectrum of the test sample and the control fingerprint spectrum is determined by whether the fingerprint spectrum of the test sample contains the peaks shown in Figures 24, 25 and / or 26. In Figure 24, the retention time and peak area of ​​each peak are shown in Table A below. Table A ； The retention time and peak area of ​​each peak in Figure 25 are shown in Table B below: Table B ； The retention time and peak area of ​​each peak in Figure 26 are shown in Table C below: Table C 。 2. The method according to claim 1, characterized in that, The similarity between the fingerprint spectrum of the sample to be tested and the control fingerprint spectrum was calculated using traditional Chinese medicine chromatography and fingerprint spectrum similarity evaluation software.

3. The method according to claim 2, characterized in that, The sample to be tested or its raw materials are considered to contain red yeast rice based on the similarity between the fingerprint spectrum of the sample to be tested and the control fingerprint spectrum being not less than 0.8 (preferably not less than 0.85; more preferably not less than 0.86; more preferably not less than 0.87; more preferably not less than 0.88; more preferably not less than 0.89; more preferably not less than 0.90).

4. The method according to claim 3, characterized in that, When the mass spectrometry conditions of the liquid chromatography-tandem triple quadrupole mass spectrometry are: a mother ion with a charge-to-mass ratio of 283.0±1 and a daughter ion with a charge-to-mass ratio of 223.0±1 are selected, the similarity between the obtained fingerprint spectrum of the test sample and Figure 24 is calculated, and the presence of red yeast rice in the test sample or its preparation raw materials is determined based on the similarity between the fingerprint spectrum of the test sample and Figure 24.

5. The method according to claim 3, characterized in that, When the mass spectrometry conditions of the liquid chromatography-tandem triple quadrupole mass spectrometry are: a mother ion with a charge-to-mass ratio of 285.0±1 and a daughter ion with a charge-to-mass ratio of 225.0±1 are selected, the similarity between the obtained fingerprint spectrum of the test sample and Figure 25 is calculated, and the presence of red yeast rice in the test sample or its preparation raw materials is determined based on the similarity between the fingerprint spectrum of the test sample and Figure 25.

6. The method according to claim 3, characterized in that, When the mass spectrometry conditions of the liquid chromatography-tandem triple quadrupole mass spectrometry are: a mother ion with a mass-to-charge ratio of 287.0±1 and a daughter ion with a mass-to-charge ratio of 227.0±1 are selected, the similarity between the obtained fingerprint spectrum of the test sample and Figure 26 is calculated, and the presence of red yeast rice in the test sample or its preparation raw materials is determined based on the similarity between the fingerprint spectrum of the test sample and Figure 26.

7. The method according to claim 3, characterized in that, A parent ion with a charge-to-mass ratio of 283.0±1 and a daughter ion with a charge-to-mass ratio of 223.0±1 were selected to obtain the first fingerprint spectrum of the sample to be tested; and A precursor ion with a charge-to-mass ratio of 285.0 ± 1 and a daughter ion with a charge-to-mass ratio of 225.0 ± 1 were selected to obtain the second fingerprint spectrum of the sample to be tested; and The parent ion with a charge-to-mass ratio of 287.0±1 and the daughter ion with a charge-to-mass ratio of 227.0±1 were selected to obtain the third fingerprint spectrum of the sample to be tested. If the similarity between the first fingerprint spectrum of the sample to be tested and Figure 24 is not less than 0.9, and the similarity between the second fingerprint spectrum of the sample to be tested and Figure 24 is not less than 0.9, and the similarity between the third fingerprint spectrum of the sample to be tested and Figure 26 is not less than 0.9, then the sample to be tested or its preparation raw materials are considered to contain red yeast rice.

8. The method according to claim 1, characterized in that, The mass spectrometry conditions for the liquid chromatography-tandem triple quadrupole mass spectrometry include: With a clustering voltage of 180V and a collision capability of 24eV, a parent ion with a charge-to-mass ratio of 283.0±1 and a daughter ion with a charge-to-mass ratio of 223.0±1 are selected. At a declustering voltage of 180V and a collisional capability of 24eV, a parent ion with a charge-to-mass ratio of 285.0±1 and a daughter ion with a charge-to-mass ratio of 225.0±1 are selected; and / or With a declustering voltage of 200V and a collision capability of 22eV, a parent ion with a charge-to-mass ratio of 287.0±1 and a daughter ion with a charge-to-mass ratio of 227.0±1 are selected.

9. The method according to claim 8, characterized in that, The mass spectrometry conditions for the liquid chromatography-tandem triple quadrupole mass spectrometry include: Ion source: Electrospray, positive ion scanning mode ESI(+); Monitoring method: MRM mode, ion source temperature 200~600℃.

10. The method according to any one of claims 1-9, characterized in that, The sample to be tested is a traditional Chinese medicine or health product.

Images