CN-120352565-B - Method for establishing fingerprint of volatile/fat-soluble component in Xinnaoning capsule

Abstract

The invention belongs to the technical field of quality detection of traditional Chinese medicine preparations, and provides a method for establishing a fingerprint of volatile/fat-soluble components in Xinnaoning capsules. The method comprises the steps of establishing a fingerprint of volatile components in the Xinnaoning capsules and establishing a fingerprint of fat-soluble components in the Xinnaoning capsules, wherein a Xinnaoning capsule medicinal preparation is taken as a detection object, and a gas chromatography and mass spectrometry combined fingerprint method is adopted to establish the fingerprint method for the medicinal preparation. The method for constructing the fingerprint of the volatile/fat-soluble component of the Xinnaoning capsule has the advantages of high stability, high precision and good repeatability. And the similarity evaluation is carried out on the fat-soluble compounds of the Xinnaoning capsules, so that technical support is provided for realizing more comprehensive and effective control of the product quality.

Inventors

• YU HUAJUN
• XIAO XUE
• TU GUOLI
• LI GUANGLI
• TIAN YAN
• LI HUILIN

Assignees

• 贵州景诚制药有限公司

Dates

Publication Date

20260508

Application Date

20250425

Claims (1)

1. 1. The method for establishing the fingerprint of the volatile/fat-soluble component in the Xinnaoning capsule is characterized by comprising the following specific steps of: establishment of fingerprint of volatile component in Xinnaoning capsule A1, preparing a test solution Weighing powder in XINNAONING Capsule, adding 10 times of water, adding 1 ml n-hexane into volatile oil collector, starting to boil, distilling to obtain volatile oil 7 h, collecting n-hexane part, and storing in small bottle to obtain small molecular volatile oil of XINNAONING Capsule; A2, GC-MS conditions The mass spectrum conditions comprise EI source with temperature of 230 ℃, four-level rod with temperature of 150 ℃, full scanning mode with scanning range of 30-550 u and auxiliary heating area with temperature of 270 ℃, solvent delay of 3 min, and searching analysis by NIST14.0 standard map; the chromatographic conditions are AGILENT HP-5MS capillary chromatographic column, the specification is 30m multiplied by 0.25m multiplied by mm m multiplied by 0.25 mu m, the temperature of a sample inlet is 250 ℃, the flow rate of the chromatographic column is 1.0ml/min, the purging flow rate of a spacer is 3 ml/min, the split ratio is 20:1, and the sample injection amount is 1 mu l; Heating to 60 deg.C for 3min deg.C/min, to 210 deg.C for 0min, and to 240 deg.C for 2 deg.C/min for 5 min; a3 measurement method Precisely sucking 1 μl of the sample solution according to GC-MS conditions, and detecting by GC-MS; Establishment of fingerprint spectrum of fat-soluble component in Xinnaoning capsule B1, preparing a test solution Weighing powder in a Xinnaoning capsule, adding ethyl acetate into the powder according to the mass volume ratio of 1:1 g/ml, carrying out ultrasonic treatment of 1h, and filtering to obtain a Xinnaoning capsule ethyl acetate solution; B2, GC-MS conditions The mass spectrum conditions comprise EI source with temperature of 230 ℃ and four-level rod with temperature of 150 ℃, full scanning mode with scanning range of 30-550 u and auxiliary heating area with temperature of 270 ℃, solvent delay of 3 min, and index analysis by NIST14.0 standard map; the chromatographic conditions are AGILENT HP-5MS capillary chromatographic column, the specification is 30m multiplied by 0.25m multiplied by mm m multiplied by 0.25 mu m, the temperature of a sample inlet is 250 ℃, the flow rate of the chromatographic column is 1.0ml/min, the purging flow rate of a spacer is 3 ml/min, the split ratio is 20:1, and the sample injection amount is 1 mu l; Heating to 60 deg.C, maintaining at 3min deg.C/min to 220 deg.C, maintaining at 5. 5min and 250 deg.C, and operating at 15 min; B3, method of measurement 1 Μl of the sample solution was precisely aspirated according to the GC-MS conditions and detected by GC-MS.

Description

Method for establishing fingerprint of volatile/fat-soluble component in Xinnaoning capsule Technical Field The invention relates to the technical field of quality detection of traditional Chinese medicine preparations, in particular to a method for establishing a fingerprint of volatile/fat-soluble components in Xinnaoning capsules. Background The Xinnaoning capsule is a product of Guizhou Jingcheng pharmaceutical limited company, is loaded in the 2020 edition of Chinese pharmacopoeia, consists of ginkgo leaf, littleleaf boxwood, red sage root, litsea coreana and longstamen onion bulb, has the functions of activating blood and promoting qi circulation, and removing obstruction in channels to relieve pain, and is clinically used for treating chest stuffiness and stinging, palpitation, dizziness and the like, and coronary heart disease and cerebral arteriosclerosis with the symptoms. At present, thin layer chromatography identification and high performance liquid chromatography are mostly adopted to carry out qualitative and quantitative identification on the effective components in the extract, such as the thin layer qualitative identification of allium macrostemon and boxwood in Xinnaoning capsule products and the high performance liquid chromatography method detection of salvianolic acid B in red sage roots. However, the Xinnaoning capsule is a compound preparation, and is prepared from five medicines, wherein the chemical components of the compound preparation are hundreds of, the types of the effective components detected by the detection method in the prior art are fewer and single, and the more comprehensive and effective quality control of the Xinnaoning capsule can not be realized. The traditional Chinese medicine fingerprint is a spectrogram or a chromatogram of chemical components of the traditional Chinese medicine obtained by means of a spectrum or chromatographic technique. The traditional Chinese medicine, especially the traditional Chinese medicine compound, contains a plurality of chemical components, and the curative effect is the overall synergistic effect, so that the reflection of the material basis cannot be illustrated from one or a plurality of components, and the illustration is needed on the whole. The traditional Chinese medicine fingerprint has the characteristics of integral, macroscopic and fuzzy analysis and the like, and the aim of integral quality control can be achieved by adopting a proper fuzzy processing mode through the description of integral characteristics. Compared with the analysis method in the prior art, the traditional Chinese medicine fingerprint technology has unique advantages in the aspects of evaluation and quality control of multi-component herbal medicines and Chinese patent medicines, and is beneficial to establishing a more accurate, comprehensive and cross-batch quality control method for the Chinese patent medicines circulating in the market at present. Therefore, fingerprint research on Xinnaoning capsule products is necessary. Disclosure of Invention The invention aims to provide a method for establishing a fingerprint of volatile/fat-soluble components in Xinnaoning capsules. In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: The invention relates to a method for establishing a volatile/fat-soluble component fingerprint in Xinnaoning capsules, which comprises the following specific steps of: establishment of fingerprint of volatile component in Xinnaoning capsule A1, preparing a test solution Weighing powder in XINNAONING Capsule, adding 8-12 times of water, adding 1ml of n-hexane into volatile oil collector, starting to time from boiling, distilling to extract volatile oil for 5-10 hr, collecting n-hexane part, and preserving in small bottle to obtain small molecular volatile oil of XINNAONING Capsule; A2, GC-MS conditions The mass spectrum condition comprises EI source with temperature of 230 deg.C, four-stage rod with temperature of 150 deg.C, full scanning mode with scanning range of 30-550u and auxiliary heating zone with temperature of 270 deg.C, solvent delay of 3min, and searching analysis by NIST14.0 standard map; The chromatographic conditions are AGILENT HP-5MS capillary chromatographic column, the specification is 30m multiplied by 0.25mm multiplied by 0.25 mu m, the temperature of a sample inlet is 240-260 ℃, the flow rate of the chromatographic column is 1.0-2.0ml/min, the flow rate of spacer purge is 3ml/min, the split ratio is 10-30:1, and the sample injection amount is 1 mu l; heating to 60 deg.C for 3min, heating to 210 deg.C at 3.5-5 deg.C/min for 0min, heating to 240 deg.C at 2-3 deg.C/min for 5min; a3 measurement method Precisely sucking 1 μl of the sample solution according to GC-MS conditions, and detecting by GC-MS; Establishment of fingerprint spectrum of fat-soluble component in Xinnaoning capsule B1, preparing a test solution Weighing powder in XINNAONING Capsule, adding eth