CN116699021A - Detection method for synchronously measuring content of borneol acetate, camphor and borneol in fructus amomi - Google Patents

Abstract

The invention provides a detection method for synchronously measuring the content of borneol acetate, camphor and borneol in fructus amomi, which comprises the steps of preparing a mother solution of a sample solution: pulverizing fructus Amomi, adding absolute ethanol, vortexing, ultrasonic treating, centrifuging, and collecting supernatant to obtain mother solution of sample solution; performing adsorption purification treatment on mother liquor of a sample solution, wherein the adsorption purification material is N-propylethylenediamine, octadecylsilane chemically bonded silica, graphitized carbon black and magnesium sulfate, and performing vortex and centrifugation after the adsorption purification treatment, and collecting supernatant to obtain a sample solution loading solution; GC-MS detection was performed. The method for synchronously measuring the borneol acetate, the camphor and the borneol in the fructus amomi by using the QuEChERS/gas-phase-mass spectrometry is established by optimizing the method for extracting and purifying the fructus amomi, and the method has the advantages of simple pretreatment, convenience and high sensitivity, and can be used for detecting and analyzing the borneol acetate, the camphor and the borneol in the fructus amomi by using the method for verifying that the method has the advantages of high yield and precision after the standard adding.

Description

A detection method for synchronous determination of borneol acetate, camphor and borneol content in amomum

technical field

The invention relates to the technical field of component detection, in particular to a detection method for synchronously measuring the contents of bornyl acetate, camphor and borneol in amomum.

Background technique

Amomum is one of the traditional Chinese "four major southern medicines". It belongs to the Zingiberaceae plant and is mainly distributed in southern provinces such as Guangdong, Hainan, Fujian, and Guangxi in China. Modern pharmacological studies have shown that amomum has good anti-ulcer, anti-diarrhea and effects of promoting gastrointestinal motility. The main medicinal ingredient of amomum is bornyl acetate. Amomum amomum, a traditional Chinese medicine, recorded in the first part of the Chinese Pharmacopoeia (2020 edition), uses traditional properties and microscopic identification to determine the authenticity of amomum, and uses the content of bornyl acetate in amomum as a quality index. Although the current "Chinese Pharmacopoeia" specified gas chromatography (GC-FID) detection method can realize the qualitative and quantitative detection of bornyl acetate in amomum, but in fact Amomum also contains pigments, fatty acids, polysaccharides, flavonoids, tannins and other components, it cannot be ruled out that their retention time on the chromatographic column is adjacent to or the same as bornyl acetate; in addition, these interfering components such as pigments, fatty acids, polysaccharides, tannins, etc. will also be enriched at the gas phase inlet, which will not only Reducing the detection sensitivity of GC-FID will also interfere with the accuracy of detection. Therefore, at present, the determination of the content of bornyl acetate is only used as the quality control index of Amomum medicinal material, and the quality standard control and detection methods need to be improved and improved.

In fact, in addition to bornyl acetate, there are other ingredients such as camphor and borneol in the volatile oil of amomum volatile oil with a content of more than 1%. Fu Chen et al. analyzed the chemical components of the volatile oil of Cinnamomum chinensis from different origins, and the results showed that the top three components with higher content in the authentic medicinal material Cinnamomum sativa were bornyl acetate, camphor, and borneol. In addition to the analgesic and anti-inflammatory effects of borneol acetate in amomum, borneol has a good effect of promoting drug absorption, and camphor has efficacies such as analgesia and sterilization. The development of multi-component identification and determination of effective medicinal ingredients such as bornyl acetate, camphor, and borneol in Amomum amomum is of great significance for the identification and quality control of Chinese herbal medicines in Amomum.

Simultaneous determination of multi-component components in amomum has also received attention. Lu Yi and others used gas chromatography (GC-FID) to detect 7 active substances such as bornyl acetate, camphor, and borneol in Amomum essential oil. Huan et al. used gas chromatography (GC-FID) combined with Fourier transform near-infrared spectroscopy (NIRS) to simultaneously determine the three medicinal components of bornyl acetate, camphor and borneol in amomum. Zhang Fang et al. used GC-FID to measure limonene, camphor, bornyl acetate, and borneol in Amomum, and HPLC to measure quercetin, epicatechin, and vanillic acid. On this basis, combined with Fourier Leaf transform infrared spectroscopy (Fourier transform infrared reflection, FTIR) and differential scanning calorimetry (Differential scanning calorimetry, DSC) established a multi-component detection fingerprint library of Amomum. Although the above methods can realize the simultaneous quantitative detection of multiple medicinal components in Amomum, the operation process is cumbersome and time-consuming.

GC-MS has full scan mode (SCAM) and selective scan (SIM) mode. The GC-MS full scan mode can scan and record the mass spectrum of ions within the specified mass range. The scanned mass range covers the mass of molecular ions and fragment ions of the tested compound, and can provide accurate mass spectra of ions and ion peaks. Mass spectrometry information such as mass, fragment ion peak intensity ratio, etc., so as to obtain the molecular weight and structure information of the compound to be tested, and perform qualitative identification through library search. This mode can be used for identifying unknowns, method development, and high-concentration analytes. Quantitative; GC-MS selective scanning mode can selectively scan specific ions for known and determined target compounds, which can obtain higher sensitivity and is suitable for trace analysis of complex samples. Gas chromatography-mass spectrometry (GC-MS) has been widely used in the separation and identification of complex components. It has the high resolution of gas phase and the high sensitivity of mass spectrometry. It is an effective tool for the qualitative and quantitative analysis of drugs and metabolites in biological samples. It is also used in the analysis of traditional Chinese medicine components.

QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample pretreatment method is a fast and convenient sample treatment method, which was originally applied to the pretreatment of various pesticide residues in vegetable and fruit matrices, and has now been widely used in food contamination However, there is no relevant report on the determination of active ingredients in Chinese herbal medicines.

Contents of the invention

In view of this, the object of the present invention is to propose a kind of detection method of bornyl acetate, camphor, borneol content in the amomum synchronously, adopt GC-MS technology in conjunction with QuEChERS pretreatment method, set up bornyl acetate in amomum , camphor, borneol effective medicinal ingredients simultaneous quantitative and qualitative detection method.

Firstly, the quantitative and qualitative characteristic ions of the target compound are determined through the full scan mode, and then the quantitative and qualitative characteristic ions of the target compound are selectively scanned and detected. Compared with the current gas phase method, GC-MS can not only provide the same retention time as the GC-FID method, but also provide mass spectrum information such as the mass spectrum of the selected ion, the accurate mass of the selected ion peak, and the intensity ratio of the fragment ion peak. Qualitatively, it is far more reliable than the GC method; quantitatively, because it does not collect quantitative characteristic ions other than non-target analytes, its quantification is more accurate. In addition, due to the use of N-propyl ethylenediamine (primary secondaryamine, PSA), octadecylsilane bonded silica gel (ostade-cylsilane, ODS or C ₁₈ ), graphitized carbon black (graphitized carbon black, GCB) and other purification The material is purified before the sample is tested on the machine. On the premise of not affecting the response of the characteristic peak of the target component to be tested, it reduces the impurities such as pigments, polysaccharides, and tannins in the sample. Enrichment not only improves detection sensitivity but also reduces instrument maintenance frequency and cost.

Technical scheme of the present invention is realized like this:

A detection method for synchronous determination of borneol acetate, camphor, and borneol content in amomum, comprising the following steps:

(1) Preparation of the mother liquor of the test solution: get the dried fruit of Amomum, pulverize, add dehydrated alcohol, vortex, sonicate, centrifuge, and collect the supernatant to obtain the mother liquor of the test solution;

(2) Preparation of the upper machine liquid of the test solution: get the mother liquor of the test solution and carry out adsorption and purification treatment, the adsorption and purification materials are N-propylethylenediamine, octadecylsilane bonded silica gel, graphitized carbon black and Magnesium sulfate, after adsorption purification treatment, vortex, centrifugation, collect supernatant, obtain the upper machine liquid of need testing solution;

(3) Preparation of mixed standard solution: get the standard items of camphor, borneol and bornyl acetate, dissolve in absolute ethanol to obtain mixed standard solution;

(4) Carry out GC-MS detection.

Amomum is the fruit of Zingiberaceae plants. In addition to being rich in volatile components such as acetylborneol ester and camphor, it also contains components such as pigments, fatty acids, polysaccharides, and tannins. The enrichment at the front end of the amomum will reduce the detection sensitivity, increase the frequency and cost of instrument maintenance, and affect the detection accuracy of the target compound. Therefore, the amomum extract needs to be purified before loading the sample for detection.

N-propyl ethylenediamine (PSA) adsorbent can absorb interference substances such as organic acid, fatty acid and sugar in the sample through _the polarity of its ethylenediamine N-propyl functional group; The non-polar effect of the octadecyl functional group bonded to the silica gel can absorb macromolecular groups such as fatty acids, olefins, sterols, and pigments with weaker polarity; Quasi-impurity has a very good effect.

Further, in step (1), according to the weight-to-volume ratio of feed to liquid: 9-12g: 20-30mL, add absolute ethanol to the crushed Amomum dried fruit, vortex for 0.5-1.5min, and use 350-400W, 50-55kHz After ultrasonic treatment for 15-25 minutes, centrifuge at 5000-6000 r/min for 8-12 minutes.

Further, in step (2), the mass ratio of N-propylethylenediamine, octadecylsilane bonded silica gel, graphitized carbon black and magnesium sulfate is 1-2:1-2:0.15-1:3 ~4.

Further, the volume-to-weight ratio of the mother liquor of the test solution to the adsorption purification material is 1-2mL: 250-350mg.

Further, in step (2), the vortex time is 0.5-1.5 min, the centrifugation speed is 10000-12000 r/min, and the centrifugation time is 3-8 min.

Further, in step (4), the gas chromatographic detection adopts temperature programming, and the temperature programming step includes the following steps: the initial column temperature is 55-65°C, kept for 0.5-1.5min, and raised to 130-170°C at 4.0-6.0°C/min, Keep it for 0.5~1.5min, and finally raise it to 260~300℃ at 25~35℃/min, and keep it for 1.5~2.5min.

Furthermore, the chromatographic column is HP-5MS, the flow rate is 0.8-1.2 mL/min, and the sampling method is split injection.

Further, in step (4), the mass spectrometry conditions are: scan time 4-16 min, scan ion range 60-160 m/z.

Furthermore, selective monitoring mode (SIM): the first scanning time is 4.0-9.5min, and the scanning ion range is 80-160m/z; the second scanning time is 9.5-12.0min, and the scanning ion range is 60-160m/z; The scanning time of the third section is 12.0～16.0min, and the scanning ion range is 90～140m/z.

Further, the electron bombardment ion source is used, the ionization energy is 65-75eV, the ion source temperature is 245-255°C, the transmission line temperature is 275-285°C, the quadrupole temperature is 145-155°C, and the solvent delay is 3.5-4.5min .

Compared with prior art, the beneficial effect of the present invention is:

The present invention establishes a method for the simultaneous determination of bornyl acetate, camphor and borneol in amomum by using QuEChERS/gas phase-mass spectrometry by optimizing the method for extracting and purifying Amomum. The method is simple, convenient and sensitive in pretreatment. Methodology verification, the recovery rate and precision of standard addition can meet the detection requirements of bornyl acetate, camphor and borneol content in amomum, and can be used for detection and analysis in amomum.

Description of drawings

Figure 1 shows the total ion current (TIC) chromatograms of three compounds (camphor, borneol, and bornyl acetate (all with a mass concentration of 10.0 μg/mL)) in SCAM scanning mode.

Figure 2 shows the recoveries of camphor, borneol, and bornyl acetate (both at a mass concentration of 10.0 μg/mL) in different purification schemes.

Fig. 3 is the selective scanning (SIM) chromatogram of camphor, borneol, bornyl acetate in the Amomum seed.

Fig. 4 is the chromatogram of the detection limit of camphor, borneol, bornyl acetate.

Fig. 5 is the chromatogram of the limit of quantification of camphor, borneol, bornyl acetate.

Detailed ways

In order to better understand the technical content of the present invention, specific examples are provided below to further illustrate the present invention.

The experimental methods used in the examples of the present invention are conventional methods unless otherwise specified.

The materials and reagents used in the examples of the present invention can be obtained from commercial sources unless otherwise specified.

16 batches of samples Amomum were purchased from the traditional Chinese medicinal materials markets in Guangdong, Guangxi and Yunnan, and were identified as the dried fruit of the perennial herbaceous plant Amomum in the family Zingiberaceae by Zhang Zhenshan, an assistant researcher at the Analysis and Testing Center of the Chinese Academy of Tropical Agricultural Sciences.

N-propylethylenediamine (PSA, 40 μm-60 μm), graphitized carbon black (GCB, 40 μm-120 μm), octadecylsilane bonded silica gel (C ₁₈ , 40 μm-60 μm, Agilent, USA).

Embodiment 1-optimization of mass spectrometry conditions

Three mixed standard solutions of camphor, borneol and bornyl acetate were prepared in absolute ethanol at 10.0 μg/mL, and scanned in full scan mode within the mass-to-charge ratio (m/z) range of 40 to 500 amu. Determine the retention time of camphor, borneol, and bornyl acetate by searching the NIST spectral library, and then select ions with high relative intensity and strong characteristics according to the compound Scan spectrum as characteristic ions, and use them as characteristic ions with large abundance values and strong characteristics The ions with high sensitivity are used as quantitative ions. The relevant parameters such as camphor, borneol, bornyl acetate retention time and characteristic ions in amomum are shown in Table 1 below. Figure 1 is the total ion current (TIC) chromatograms of three compounds of camphor, borneol and bornyl acetate with a mass concentration of 10.0 μg/mL.

Table 1 camphor, borneol, bornyl acetate selective scanning (SIM) characteristic ion parameters

Example 2 - Sample Preparation

Take the mature dried amomum fruit (Zingiberaceae Cardamom plant Yangchunsha), pulverize it with a powder machine, prepare dry powder, pass through a No. 3 sieve, seal it in a bag, and store it in a desiccator for future use.

Preparation of the mother liquor of the test solution: Accurately weigh 10.00g (accurate to 0.01g) of the powder of this product, place it in a 50mL centrifuge tube with stopper, accurately add 25.0mL of absolute ethanol (accurate to 0.1mL), seal it tightly, weigh Determine the weight, vortex for 1min, sonicate (350W, 53kHz) for 20min, let it cool; make up the lost weight with absolute ethanol, shake well, then centrifuge at 5000r/min for 10min, suck the supernatant, and get the test product solution mother liquor.

Preparation of the upper machine solution of the test solution: accurately draw 1.5mL of the mother solution and place it in the QuEChERS dispersive purification reagent tube, which contains adsorption and purification materials including N-propylethylenediamine (PSA), C ₁₈ , graphitized carbon black (GCB), Vortex for 1 min, and then centrifuge at 10,000 r/min for 5.0 min; absorb the supernatant with a disposable syringe, and pass through a 0.22 μm organic filter membrane to obtain the supernatant of the test solution.

The four purification schemes are as follows:

①50mg PSA+150mg MgSO ₄ ;

②50mg PSA+50mg C ₁₈ +150mg MgSO ₄ ;

③50mg PSA+50mg C ₁₈ +7.5mg GCB+150mg MgSO ₄ ;

④50mg PSA+50mg C ₁₈ +50mg GCB+150mg MgSO ₄ .

Prepare 10.0 μg/mL 3 mixed standard solutions of camphor, borneol, and bornyl acetate, and absorb 1.5mL of the mixed standard solution and add it to the above 4 kinds of purification material systems for detection after purification treatment. Six parallel samples were made for each scheme, and the purification effects of different schemes were investigated through the average recovery rate.

The results are shown in Table 2 and Fig. 2, and the results show that the recovery rates are all in the range of 94.5% to 100%, that is, PSA, C ₁₈ and GCB have no obvious adsorption to the above-mentioned 3 compounds.

Table 2 The recoveries of camphor, borneol, bornyl acetate in different purification schemes

In the actual process of sample processing, the color of schemes ① and ② is tea-yellow. With the addition of GCB, the color of the purified sample becomes lighter yellow, and the color is clear and transparent, indicating that GCB has an adsorption effect on the pigment in the sample, and the purification effect of the sample is better. .

Embodiment 3-instrument conditions

7890B-5977A single quadrupole gas chromatography mass spectrometer (Agilent, USA).

The instrument conditions are as follows:

Chromatographic conditions: HP-5MS chromatography (30mm×0.25mm×0.25μm, Agilent, USA);

Program temperature increase: initial column temperature is 60°C, keep for 1.0min, raise to 150°C at 5.0°C/min, keep for 1.0min; finally rise to 280°C at 30°C/min, keep for 2.0min; total running time is 26.33min. The carrier gas was high-purity He (purity ≥ 99.999%), the flow rate was 1.0 mL/min; the injection volume was 1.0 μL; the injection method was split injection, and the split ratio was 20:1.

Mass spectrometry conditions: electron bombardment (EI) ion source, ionization energy 70eV; ion source temperature 250°C; transfer line temperature 280°C; quadrupole temperature 150°C; solvent delay 4.0min; selective monitoring mode (SIM): the first stage Scan time 4.0～9.5min, scan ions 81, 95, 108, 152; second scan time 9.5～12.0min, scan ions 67, 95, 110, 152; third scan time 12.0～16.0min, scan ions 95 , 108, 121, 136.

The results are shown in Figure 3.

Embodiment 4-methodological investigation

(1) Linear range and detection limit of the method

Camphor, borneol, and bornyl acetate were prepared with absolute ethanol as the corresponding standard working solutions. In this series of solutions, the concentrations of camphor were 50, 100, 200, 500, 1000, and 2000 μg/mL; The concentrations of brain were 5, 10, 20, 50, 100, 200 μg/mL; the concentrations of bornyl acetate were 100, 200, 500, 1000, 2000, 5000 μg/mL, respectively.

Measured under optimized instrument conditions, take the peak area y of the quantitative ion of the target compound to be measured as the ordinate, and the mass concentration x (μg/kg) as the abscissa, and make a standard curve to obtain camphor, borneol, and bornyl acetate The linear equations and correlation coefficients of the three targets. The results show that the three target analytes of camphor, borneol and bornyl acetate have a good linear relationship with the peak area corresponding to the response within the measured mass concentration range (r ² ≧0.997). The corresponding linear regression equation and correlation coefficient are shown in the table 2.

Add the mixed standard solution of camphor, borneol, and bornyl acetate in absolute ethanol, and use the stepwise dilution method to detect on the machine. Use the software that comes with the instrument to calculate the signal-to-noise ratio, and use 3 times the signal-to-noise ratio (S/N≧ 3) Calculate the limit of detection (LOD) of the method, calculate the limit of quantitation (LOQ) of the method with 10 times the signal-to-noise ratio (S/N≧10), and then get the corresponding limit of detection of the sample solution on the machine of this method They are 0.002μg/mL (Figure 4) and quantification limit 0.005μg/mL (Figure 5); in this method, 10.0g sample is weighed and placed in 25.0mL absolute ethanol for extraction, then the detection limit of this method is 0.002μg/mL mL×25.0mL/10.0g=0.005mg/kg; the limit of quantification is 0.005μg/mL×25.0mL/10.0g=0.012mg/kg.

Table 2 camphor, borneol, bornyl acetate linear range, linear equation, correlation coefficient, detection limit and limit of quantification

(2) Inspection of precision

Draw 10.0 μg/mL camphor, borneol, and bornyl acetate mixed standard solutions for six consecutive injections according to the optimized instrument method, each injection volume is 0.1 μL, record the peak area, calculate the precision, and the RSD value is 2.3% (n=7), indicating good instrument precision.

(3) Stability inspection

Draw the prepared sample solution for inspection, and inject samples according to the above-mentioned instrument method conditions, respectively inject samples at 0, 1, 2, 4, 8, 16, and 24 hours after preparation, the sample injection volume, and the RSD of the measurement results is 2.6%. Indicates that the sample is relatively stable within 24 hours.

(4) Repeated inspection

Take the same batch of amomum samples, prepare 6 samples on the machine at the same time according to the preparation method of the test sample solution, and measure them according to the above-mentioned optimized conditions. The average mass concentrations of camphor, borneol, and bornyl acetate in the measured samples were 0.373mg/g, 5.22mg/g, and 11.1mg/g, respectively, and the corresponding relative standard deviations RSD were: 2.1%, 3.2%, 3.3 %, indicating that the reproducibility of this method is relatively good.

Background content of camphor, borneol and bornyl acetate in Table 3 Amomum

(5) The recovery rate and precision of the method

Additive recovery and precision experiments were performed. Accurately weigh 10.00g (accurate to 0.01g) blank sample, 6 samples each with camphor concentration of 5.0, 10.0, and 20.0mg/g, and 6 samples each with borneol concentration of 0.50, 1.0, and 2.0mg/g , 6 samples each with concentrations of 10.0, 20.0, and 40.0 mg/g of bornyl acetate were added, and the recovery rate experiment was carried out, and the average recovery rate and relative standard deviation were calculated to investigate the accuracy and precision of the method, as shown in Table 4 . The results showed that the recoveries of camphor, borneol, and bornyl acetate were between 98.0% and 105%, and the relative standard deviation (RSD) was between 1.3% and 3.1%, which met the methodological requirements. .

The average recovery and relative standard deviation of camphor, borneol, bornyl acetate in table 4 Amomum

In summary, the present invention has established a method for the simultaneous determination of bornyl acetate, camphor, and borneol in Amomum amomum by QuEChERS/gas phase-mass spectrometry by optimizing the method for extracting and purifying Amomum, and the pretreatment of the method is simple and convenient , High sensitivity, through methodological verification, the recovery rate, precision, minimum detection limit and limit of quantification of standard addition can meet the detection requirements of bornyl acetate, camphor and borneol content in amomum, and can be used for detection and analysis in amomum . The establishment of this method improves the analysis and detection technology for the simultaneous determination of bornyl acetate, camphor and borneol in amomum, and is of great significance for improving the quality and safety of amomum products and ensuring the healthy development of amomum industry.

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the scope of the present invention. within the scope of protection.

Claims (10)

1. a kind of detection method of bornyl acetate, camphor, borneol content in the amomum synchronously measured, is characterized in that, comprises the following steps: (1) Preparation of the mother liquor of the test solution: get the dried fruit of Amomum, pulverize, add dehydrated alcohol, vortex, sonicate, centrifuge, and collect the supernatant to obtain the mother liquor of the test solution; (2) Preparation of the upper machine liquid of the test solution: get the mother liquor of the test solution and carry out adsorption and purification treatment, the adsorption and purification materials are N-propylethylenediamine, octadecylsilane bonded silica gel, graphitized carbon black and Magnesium sulfate, after adsorption purification treatment, vortex, centrifugation, collect supernatant, obtain the upper machine liquid of need testing solution; (3) Preparation of mixed standard solution: get the standard items of camphor, borneol and bornyl acetate, dissolve in absolute ethanol to obtain mixed standard solution; (4) Carry out GC-MS detection. 2. the detection method of borneol acetate, camphor, borneol content in synchronous determination amomum according to claim 1, is characterized in that, in step (1), be 9～12g by feed liquid weight volume ratio: 20 ～30mL, add absolute ethanol to the crushed amomum dried fruit, vortex for 0.5～1.5min, perform ultrasonic treatment at 350～400W, 50～55kHz for 15～25min, then centrifuge at 5000～6000r/min for 8～12min. 3. the detection method of borneol acetate, camphor, borneol content in synchronous measurement amomum according to claim 1, is characterized in that, in step (2), N-propyl ethylenediamine, octadecyl The mass ratio of silane-bonded silica gel, graphitized carbon black and magnesium sulfate is 1-2:1-2:0.15-1:3-4. 4. the detection method of borneol acetate, camphor, borneol content in synchronous measurement amomum according to claim 1, is characterized in that, the material-liquid volume-to-weight ratio of need testing solution mother liquor and adsorption purification material is 1～ 2mL: 250~350mg. 5. the detection method of bornyl acetate, camphor, borneol content in synchronous measurement amomum according to claim 1 is characterized in that, in step (2), vortex time is 0.5～1.5min, and centrifugal speed is 10000～12000r/min, the centrifugation time is 3～8min. 6. the detection method of borneol acetate, camphor, borneol content in synchronous measurement amomum according to claim 1, is characterized in that, in step (4), gas chromatography detection adopts programmed temperature rise, and programmed temperature rise step comprises as follows : The initial column temperature is 55-65°C, keep it for 0.5-1.5min, raise it to 130-170°C at 4.0-6.0°C/min, keep it for 0.5-1.5min, and finally raise it to 260-300°C at 25-35°C/min, Keep it for 1.5-2.5 minutes. 7. the detection method of synchronous determination borneol acetate, camphor, borneol content in amomum according to claim 6, is characterized in that, chromatographic column is HP-5MS, and flow velocity is 0.8～1.2mL/min, sample injection The method is split injection. 8. the detection method of synchronously measuring borneol acetate, camphor, borneol content in amomum according to claim 1, is characterized in that, in step (4), mass spectrometry condition is: scan time 4～16min, scan ion The range is 60~160m/z. 9. The method for synchronously measuring borneol acetate, camphor, and borneol content in amomum according to claim 8, characterized in that, selective monitoring mode: the first scan time is 4.0 to 9.5 min, and the ion range is scanned 80~160m/z; the second scanning time is 9.5~12.0min, and the scanning ion range is 60~160m/z; the third scanning time is 12.0~16.0min, and the scanning ion range is 90~140m/z. 10. the detection method of borneol acetate, camphor, borneol content in synchronous measurement amomum according to claim 8 is characterized in that, adopts electron bombardment ion source, ionization energy is 65～75eV, and ion source temperature is 245-255°C, transfer line temperature 275-285°C, quadrupole temperature 145-155°C, solvent delay 3.5-4.5min.