A method for detecting multiple components in zedoary turmeric oil

Abstract

The invention relates to a method for detecting the content of multiple components in zedoary turmeric oil, and belongs to the technical field of quality control of traditional Chinese medicine. The detection method of the invention can simultaneously detect the contents of 8 components in zedoary turmeric oil, has high separation, the minimum separation between two adjacent component peaks is greater than 1.5, has good linearity, the linear correlation coefficient of each component reaches more than 0.999, has high accuracy, good precision, good solution stability, the solution is stable within 24 hours at room temperature, has good durability, greatly improves work efficiency and detection accuracy, and has positive significance for improving the quality standard of zedoary turmeric oil.

Description

Technical Field

[0001] The invention relates to a method for detecting multiple components in zedoary turmeric oil, and belongs to the technical field of quality control of traditional Chinese medicines. Background Art

[0002] Curcuma oil injection has a direct inhibitory or killing effect on respiratory viruses and influenza viruses, and also has an inhibitory effect on Staphylococcus aureus, Escherichia coli and Salmonella typhi. It is clinically used for the treatment of upper respiratory tract infections, pneumonia, enteritis, myocarditis, encephalitis, tumors and anti-thrombotic symptoms caused by viruses. The main adverse reactions in clinical practice include allergic reactions, respiratory and circulatory system reactions, and digestive system reactions.

[0003] Curcuma oil is a volatile oil extracted from the warm zedoaria by steam distillation. Its main components are curdione, geranone, curcumene, and furadiene, which have been included in the 2020 edition of the Chinese Pharmacopoeia. The pharmacopoeia only stipulates the content of geranone and furadiene. Testing only the content of these two components cannot fully control the quality of zedoaria oil. Therefore, it is necessary to test the content of more components to improve the quality control level of zedoaria oil. Summary of the invention

[0004] The purpose of the present invention is to overcome the deficiencies of the above-mentioned prior art and provide a method for detecting multiple components in zedoary oil. The detection method can detect the contents of more components, which is of great significance for improving the quality control of zedoary oil.

[0005] To achieve the above object, the technical solution adopted by the present invention is: a method for detecting multiple components in zedoary oil, the detection method comprising the following steps:

[0006] (1) Preparation of test solution: Prepare zedoary turmeric oil with ethanol to obtain an ethanol solution of zedoary turmeric oil;

[0007] (2) Preparation of reference solution: α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol, and β-elemene were prepared into solutions with ethanol;

[0008] (3) Gas chromatography detection: The following temperature program is used: initial temperature 115-125°C, holding time 0 min, then heating to 165-175°C, holding time 0 min, then heating to 240-250°C, holding time 15-17 min. This temperature program can achieve baseline separation of the detected components and meet the content detection requirements.

[0009] By adopting the detection method of the present invention, it can be ensured that α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol and β-elemene in zedoary turmeric oil reach baseline separation within 44 minutes, and the peak separation of each component meets the content measurement requirement with high accuracy, so that the present invention can monitor the contents of 8 components in zedoary turmeric oil with high sensitivity and high efficiency.

[0010] Furthermore, the above-mentioned method for detecting the contents of various components in zedoary oil can be used for quality monitoring of zedoary oil.

[0011] As a preferred embodiment of the detection method of the present invention, in the step (1), the concentration of the ethanol solution of Curcuma oil is 0.5-1.5 mg / mL.

[0012] As a preferred embodiment of the detection method of the present invention, in the step (2), the concentration of the solution prepared by using ethanol is 0.02-0.04 mg / mL.

[0013] As a preferred embodiment of the detection method of the present invention, in the step (3), the gas chromatography detection adopts the automatic sampling method, and the gas chromatography column model adopted is: ZB-624 gas chromatography column produced by Phenomenex Inc. with a particle size of 60m*0.25mm and 1.4um.

[0014] As a preferred embodiment of the detection method of the present invention, in step (3), the injection volume of the test solution and the reference solution is 1 μL.

[0015] As a preferred embodiment of the detection method of the present invention, in the step (3), the injection port temperature is 190-210°C, the split ratio is 8:1-12:1, the detector temperature is 240-260°C, the nitrogen flow rate is 25-35 mL / min, the hydrogen flow rate is 25-35 mL / min, and the air flow rate is 280-320 mL / min.

[0016] As a preferred embodiment of the detection method of the present invention, the injection port temperature is 200°C, the detector temperature is 250°C, the nitrogen flow rate is 30 mL / min, the hydrogen flow rate is 30 mL / min, and the air flow rate is 300 mL / min.

[0017] As a preferred embodiment of the detection method of the present invention, in step (3), the gas chromatography detection includes: injecting the reference solution and the test solution into the gas chromatograph for measurement, recording the data, and then calculating the content of each component using the external standard method.

[0018] As a preferred embodiment of the detection method of the present invention, in the step (3), the heating rate to 165-175°C is 1.8-2.2°C / min; the heating rate to 240-250°C is 18-22°C / min.

[0019] As a preferred embodiment of the detection method of the present invention, the following temperature rise program is adopted: initial temperature 115-125°C, holding time 0 min, then heating to 165-175°C, holding time 0 min, then heating to 240-250°C, holding time 15-17 min. This temperature rise program can achieve baseline separation of the detected components and meet the content detection requirements.

[0020] Compared with the prior art, the invention has the following beneficial effects: the detection method of zedoary turmeric oil of the invention can detect the contents of 8 components in zedoary turmeric oil, and improves the quality control level of zedoary turmeric oil. The invention can simultaneously detect the contents of 8 components in zedoary turmeric oil, has high separation, the minimum separation between two adjacent component peaks is greater than 1.5, has good linearity, the linear correlation coefficient of each component reaches more than 0.999, has high accuracy, the recovery rate meets the content detection requirements, has good precision, has good solution stability, the solution is stable within 24 hours at room temperature, has good durability, greatly improves work efficiency and detection accuracy, and has positive significance for improving the quality standard of zedoary turmeric oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is the gas chromatogram of the reference substance in Example 1. DETAILED DESCRIPTION

[0022] In order to better illustrate the purpose, technical solutions and advantages of the present invention, the present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

[0023] Unless otherwise specified, the experimental methods used in the examples of the present invention are all conventional methods. The materials, reagents, etc. used in the examples of the present invention, unless otherwise specified, can all be obtained from commercial channels.

[0024] Example 1

[0025] A method for detecting multiple components in zedoary turmeric oil, characterized in that the detection method comprises the following steps:

[0026] (1) Preparation of test solution: Curcuma oil was prepared with ethanol to obtain a 1 mg / mL ethanol solution of Curcuma oil;

[0027] (2) Preparation of reference solution: α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol, and β-elemene were prepared into 0.03 mg / mL solutions in ethanol;

[0028] (3) Gas chromatography detection: The following heating program was used: initial temperature 120 °C, holding time 0 min, then heating to 170 °C at a rate of 2 °C / min, holding time 0 min, then heating to 245 °C at a rate of 20 °C / min, holding time 16 min;

[0029] The automatic injection method was adopted, and the gas chromatography column model used was: ZB-624 gas chromatography column produced by Phenomenex Inc. with a particle size of 60m*0.25mm and 1.4um. 1μL of the test solution and the reference solution were respectively drawn, the injection port temperature was 200℃, the split ratio was 10:1, the detector temperature was 250℃, the nitrogen flow rate was 30mL / min, the hydrogen flow rate was 30mL / min, and the air flow rate was 300mL / min; the reference solution and the test solution were injected into the gas chromatograph for determination, and the data were recorded, and then the content of each component was calculated by the external standard method.

[0030] The reference solution was used to locate each component in the test sample, and the content of each component was calculated by the external standard method, as shown in Table 1.

[0031] Table 1

[0032]

[0033]

[0034] Example 2

[0035] A method for detecting multiple components in zedoary turmeric oil, characterized in that the detection method comprises the following steps:

[0036] (1) Preparation of test solution: Curcuma oil was prepared with ethanol to obtain a 0.5 mg / mL ethanol solution of Curcuma oil;

[0037] (2) Preparation of reference solution: α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol, and β-elemene were prepared into 0.02 mg / mL solutions in ethanol;

[0038] (3) Gas chromatography detection: The following heating program was used: initial temperature 115 °C, holding time 0 min, then heating to 175 °C at a rate of 1.8 °C / min, holding time 0 min, then heating to 250 °C at a rate of 18 °C / min, holding time 15 min;

[0039] Automatic injection method was adopted, and the gas chromatography column model used was: ZB-624 gas chromatography column produced by Phenomenex Inc. with a particle size of 60m*0.25mm and 1.4um. 1μL of test solution and reference solution were respectively drawn, the injection port temperature was 190℃, the split ratio was 8:1, the detector temperature was 240℃, the nitrogen flow rate was 25mL / min, the hydrogen flow rate was 25mL / min, and the air flow rate was 280mL / min. The reference solution and the test solution were injected into the gas chromatograph for determination, and the data was recorded. Then, the content of each component was calculated by the external standard method.

[0040] The reference solution was used to locate each component in the test sample, and the content of each component was calculated by the external standard method, as shown in Table 2.

[0041] Table 2

[0042]

[0043]

[0044] Example 3

[0045] A method for detecting multiple components in zedoary turmeric oil, characterized in that the detection method comprises the following steps:

[0046] (1) Preparation of test solution: Curcuma oil was prepared with ethanol to obtain a 1.5 mg / mL ethanol solution of Curcuma oil;

[0047] (2) Preparation of reference solution: α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol, and β-elemene were prepared into 0.04 mg / mL solutions in ethanol;

[0048] (3) Gas chromatography detection: The following heating program was used: initial temperature 125 °C, holding time 0 min, then heating to 165 °C at a rate of 2.2 °C / min, holding time 0 min, then heating to 240 °C at a rate of 22 °C / min, holding time 17 min;

[0049] Automatic sampling method was adopted, and the gas chromatography column model used was: ZB-624 gas chromatography column produced by Phenomenex Inc. with a particle size of 60m*0.25mm and 1.4um. 1μL of test solution and reference solution were respectively drawn, the injection port temperature was 210℃, the split ratio was 12:1, the detector temperature was 260℃, the nitrogen flow rate was 35mL / min, the hydrogen flow rate was 35mL / min, and the air flow rate was 320mL / min. The reference solution and the test solution were injected into the gas chromatograph for determination, and the data was recorded. Then, the content of each component was calculated by the external standard method.

[0050] The reference solution was used to locate each component in the test sample, and the content of each component was calculated by the external standard method, as shown in Table 3.

[0051] Table 3

[0052]

[0053]

[0054] Example 4 Linearity Test

[0055] Take mixed reference solution, press the chromatographic condition of embodiment 1, prepare linear concentration solution, calculate peak area and linear correlation coefficient, the result shows that α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol, β-elemene are within the linear range, the linear correlation coefficient is greater than 0.999, and the linear relationship is good. Specific as shown in Table 4.

[0056] Table 4

[0057]

[0058]

[0059] Example 5 Precision Test

[0060] Six test solutions were prepared and tested according to the method of Example 1. The chromatographic peak area and acid RSD were recorded. The results showed that the RSD of α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol, and β-elemene in the test solution were all less than 5%, with good repeatability. The details are shown in Table 5.

[0061] Table 5

[0062] name Retention time (min) RSD(%) α-Pinene 10.585 4.4 Camphene 11.378 4.5 β-pinene 12.411 4.7 1,8-Cineole 14.780 4.7 Linalool 18.335 4.6 Camphor 22.912 4.5 Isoborneol 23.238 3.7 β-elemene 29.508 4.8

[0063] Example 6 Stability Test

[0064] The test solution was taken at 0h and after 24h of placement, and the results showed that after the test solution was placed for 24h, the peak areas of α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol, and β-elemene were all recovered at 98.0% to 102.0% compared with 0h. The stability of the test solution within 24h of placement is shown in Table 6.

[0065] Table 6

[0066] name Peak area at 0h 24h peak area Recovery rate (%) α-Pinene 115.599 114.979 99.5％ Camphene 191.086 192.682 100.8％ β-pinene 119.679 120.061 100.3％ 1,8-Cineole 1198.750 1212.076 101.1％ Linalool 136.651 137.237 100.4％ Camphor 310.752 312.385 100.5％ Isoborneol 187.840 190.195 101.3％ β-elemene 823.390 832.088 101.1％

[0067] Example 7 Solution Durability Test

[0068] According to the detection method of Example 1, the original column flow rate of 1.5 mL / min was adjusted to 1.4 mL / min and 1.6 mL / min, respectively, to detect the content of the same batch of test solutions. The results showed that when the column flow rate was changed, the RSDs of the contents of α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol and β-elemene were all within 5%, and the method had good durability, as shown in Table 7.

[0069] Table 7

[0070]

[0071]

[0072] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A method for detecting multiple components in zedoary turmeric oil, characterized in that: The detection method comprises the following steps: (1) Preparation of test solution: Prepare zedoary ... (2) Preparation of reference solution: prepare solutions of α-pinene, camphene, β-pinene, 1,8-cineole, linalool, camphor, isoborneol and β-elemene respectively with ethanol; (3) Gas chromatography detection: The following heating program was used: initial temperature 115~125℃, holding time 0min, then heating to 165~175℃, holding time 0min, then heating to 240~250℃, holding time 15~17min; In the step (3), the gas chromatography detection adopts the automatic sampling method, and the gas chromatography column model adopted is: ZB-624 gas chromatography column with a particle size of 60m*0.25mm and 1.4um produced by Phenomenex Inc.; In the step (3), the injection port temperature is 190-210°C, the split ratio is 8:1-12:1, the detector temperature is 240-260°C, the nitrogen flow rate is 25-35 mL / min, the hydrogen flow rate is 25-35 mL / min, and the air flow rate is 280-320 mL / min; In the step (3), the heating rate to 165-175°C is 1.8-2.2°C / min; the heating rate to 240-250°C is 18-22°C / min.

2. The detection method according to claim 1, characterized in that In the step (1), the concentration of the ethanol solution of Curcuma oil is 0.5-1.5 mg / mL.

3. The detection method according to claim 1, characterized in that In the step (2), the concentration of the solution prepared by using ethanol is 0.02-0.04 mg / mL.

4. The detection method according to claim 1, characterized in that In step (3), the injection volume of the test solution and the reference solution is 1 μL.

5. The detection method according to claim 1, characterized in that The injection port temperature was 200 °C, the detector temperature was 250 °C, the nitrogen flow rate was 30 mL / min, the hydrogen flow rate was 30 mL / min, and the air flow rate was 300 mL / min.

6. The detection method according to claim 1, characterized in that In the step (3), the gas chromatography detection includes: injecting the reference solution and the test solution into the gas chromatograph for measurement, recording the data, and then calculating the content of each component using the external standard method.

7. The detection method according to claim 1, characterized in that: The following heating program was adopted: initial temperature 120°C, holding time 0 min, then heating to 170°C at a rate of 2°C / min, holding time 0 min, then heating to 245°C at a rate of 20°C / min, holding time 15 min.

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