CN-121994967-A - GC method for rapidly identifying rhizoma dryopteris crassirhizomae and counterfeits thereof

Abstract

The invention belongs to the technical field of medicine detection, and particularly provides a GC method for rapidly identifying rhizoma dryopteris crassirhizomae and counterfeits thereof, and particularly discloses application of trans-nerolidol in identifying or assisting in identifying rhizoma dryopteris crassirhizomae and counterfeits thereof, wherein the trans-nerolidol is extremely high in sample content of the rhizoma dryopteris crassirhizomae and relatively low in other counterfeits of the rhizoma dryopteris crassirhizomae, can be used as a marker of the rhizoma dryopteris crassirhizomae, establishes a method for identifying the rhizoma dryopteris crassirhizomae, has relatively good linear relation, has good specificity, instrument precision, stability, repeatability and reproducibility, has a quantitative limit of 0.139 mug/ml, a detection limit of 0.046 mug/ml, the trans-nerolidol content of 32 mass samples is between 0.11% -1.39%, and the trans-nerolidol content of rhizoma dryopteris not less than 0.25%, and provides a more accurate method for identifying and controlling quality of the rhizoma dryopteris provided.

Inventors

• LIN RUILI
• LIU SHENGCAI
• SUO JUN
• Mao Yaojie
• DONG WENTAO
• ZHOU LIHUA
• WANG LIMEI
• Liu bailong
• WANG YALI
• ZHANG MINGTONG
• YONG FENG
• MA XIAO
• JIN WANJUN
• LAI JING
• XU NING
• MA LIYA
• SHI XIAOYA

Assignees

• 甘肃省药品检验研究院

Dates

Publication Date

20260508

Application Date

20260310

Claims (10)

1. 1. The application of trans-nerolidol in identifying or assisting in identifying rhizoma dryopteris crassirhizomae and rhizoma dryopteris crassirhizomae pseudo products.
2. 2. Application of trans-nerolidol in preparing product for identifying or assisting in identifying rhizoma Dryopteris Crassirhizomatis and rhizoma Dryopteris Crassirhizomatis pseudo products.
3. 3. The application of trans-nerolidol in identifying or assisting in identifying whether rhizoma dryopteris crassirhizomae contains rhizoma dryopteris crassirhizomae pseudo products.
4. 4. Application of trans-nerolidol in preparing and identifying or assisting in identifying whether rhizoma dryopteris crassirhizomae pseudo products are contained in rhizoma dryopteris crassirhizomae samples.
5. 5. Application of trans-nerolidol in preparing a false product for identifying or assisting in identifying whether rhizoma dryopteris crassirhizomae is adulterated or not.
6. 6. The use according to any one of claims 1 to 5, wherein said rhizoma Dryopteris Crassirhizomatis counterfeit product comprises one or more of Su Tiejue, rhizoma Osmundae and rhizoma Cannabifoliae.
7. 7. The identification method of the rhizoma dryopteris crassirhizomae is characterized by comprising the following steps of: (1) Preparation of a control solution: Taking a proper amount of trans-nerolidol reference substance, precisely weighing, and adding ethyl acetate to prepare a solution containing 0.09 mg in each 1 ml part; (2) Preparation of test solution: Precisely weighing the sample fine powder, placing into conical flask with plug, precisely adding 25-35ml of extraction solvent, sealing, weighing, heating, reflux extracting or ultrasonic extracting, cooling, weighing again, supplementing weight loss with ethyl acetate, shaking, filtering, and collecting filtrate; (3) Detection of Taking the reference substance solution prepared in the step (1) and the sample solution prepared in the step (2) respectively for determination, wherein the chromatographic conditions are as follows: The temperature programming is that the initial temperature is 60 ℃, 5min is kept, the temperature is increased to 90 ℃ at the rate of 10 ℃ per minute, 10 min is kept, the temperature is increased to 160 ℃ at the rate of 10 ℃ per minute, 20 min is kept, the temperature is increased to 280 ℃ at the rate of 5 ℃ per minute, 10 min is kept, the temperature is increased to 300 ℃ at the rate of 20 ℃ per minute, 20 min is kept, or The temperature programming is that the initial temperature is 60 ℃, the temperature is kept 5min, the temperature is raised to 90 ℃ at the rate of 10 ℃ per minute, the temperature is kept 10min, the temperature is further raised to 160 ℃ at the rate of 10 ℃ per minute, the temperature is kept 20 min, the temperature is further raised to 250 ℃ at the rate of 10 ℃ per minute, the temperature is kept 5min, or Temperature programming, namely, the initial temperature is 70 ℃ and kept for 2 minutes, the temperature is increased to 180 ℃ at the rate of 15 ℃ per minute and kept for 25 minutes; The temperature of the sample inlet is 230 ℃ and the temperature of the detector is 250 ℃; The split ratio was 5:1, and the column flow rate was 1.5ml/min.
8. 8. The method according to claim 7, wherein the extraction solvent in the step (2) is one or more of ethyl acetate, cyclohexane, dichloromethane and n-hexane.
9. 9. The method of claim 7, wherein the chromatographic conditions of step (3) are programmed to an initial temperature of 70℃for 2 minutes and a temperature of 15℃per minute to 180℃for 25 minutes.
10. 10. The identification method of claim 7, wherein the extraction in step (2) is ultrasonic extraction for 90 minutes.

Description

GC method for rapidly identifying rhizoma dryopteris crassirhizomae and counterfeits thereof Technical Field The invention belongs to the technical field of medicine detection, and particularly relates to a GC method for rapidly identifying rhizoma dryopteris crassirhizomae and counterfeits thereof. Background Rhizoma Dryopteris Crassirhizomatis (Dryopteris crassirhizoma) is dry rhizome and petiole residue of Dryopteris crassifolia (Dryopteris crassirhizoma Nakai) of Dryopteridaceae, and is a traditional Chinese medicine with long history, wide application and quite characteristics. Rhizoma dryopteris crassirhizomae belongs to traditional Chinese medicine cyrtomium crassifolium, but the constitution of cyrtomium crassifolium is complex, and the literature reports that the number of cyrtomium crassifolium is not less than 35, and belongs to 6 families 12. In the dictionary of Chinese medicine, 7 basic plants of cyrtomium fortunei are recorded. Wherein, dryopteris crassifolia (Dryopteris crassifolia Nakai.) is the main basic plant of cyrtomium fortunei, and the collection varieties of cyrtomium fortunei in Chinese pharmacopoeia are cyrtomium fortunei and cyrtomium fortunei. Rhizoma Dryopteris Crassulae (Dryopteris Crassulaceae Nakai) and rhizoma Osmundae (Osmunda japonica Thunb.) 2 are described in the pharmacopoeia of the people's republic of China (hereinafter referred to as "pharmacopoeia") 1977 edition, and rhizoma Dryopteris Crassulae is listed in single column from "pharmacopoeia" 1995 edition to distinguish rhizoma Dryopteris from other basic plants. The traditional Chinese medicine composition is complex, is easily influenced by the production place, the processing method and the harvesting time, and has important significance for guaranteeing the safety and effectiveness of clinical medication and establishing a scientific and reasonable quality evaluation mode for controlling the overall quality of the traditional Chinese medicine. Rhizoma dryopteris crassirhizomae is the most widely used variety with the largest sales in the market, but quality control is limited to conventional projects such as properties, thin-layer identification, extract measurement and the like, and quality control standards are relatively lagged. The clinical use of cyrtomium fortunei is not always cyrtomium fortunei, and through long-term examination and market standardization, more than 5 kinds of plant rhizomes are still used as cyrtomium fortunei in the market at present, namely, conventional single bud bristlegrass fern (Woodwardia unigemmata Naka) of the Umbelliferae family, bristlegrass fern (Woodwardia japonica Sm) of the Umbelliferae family, pod fern (Matteuccias truthipteris Todaro) of the Umbelliferae family, moth fern (Lunathyriuma crostichoides Ching) of the Umbelliferae family and fakery fern Su Tiejue (Braainia insignis J.Sm) of the Umbelliferae family. They are very similar in appearance and morphological characteristics to rhizoma dryopteris crassirhizomae, and the non-identified person with abundant experience cannot be accurately identified in a sensory way. Therefore, the establishment of a rapid and accurate complementary inspection method for identifying the rhizoma dryopteris crassirhizomae, other conventional products and adulterated products has important clinical significance. Disclosure of Invention The primary purpose of the invention is to provide the application of trans-nerolidol in the identification or auxiliary identification of rhizoma dryopteris crassirhizomae pseudo-products. The second purpose of the invention is to provide an application of trans-nerolidol in preparing a product for identifying or assisting in identifying rhizoma dryopteris crassirhizomae and rhizoma dryopteris crassirhizomae pseudo products. The third purpose of the invention is to provide an application of trans-nerolidol in identifying or assisting in identifying whether rhizoma dryopteris crassirhizomae contains rhizoma dryopteris crassirhizomae pseudo products. The fourth purpose of the invention is to provide an application of trans-nerolidol in preparing a product for identifying or assisting in identifying whether rhizoma dryopteris crassirhizomae pseudo-product is contained in a rhizoma dryopteris crassirhizomae sample. The fifth purpose of the invention is to provide an application of trans-nerolidol in preparing a false product for identifying or assisting in identifying whether rhizoma dryopteris crassirhizomae is adulterated or not. Preferably, the rhizoma dryopteris crassirhizomae pseudo product comprises one or more of Su Tiejue, rhizoma Osmundae and single bud bristled fern. The sixth object of the invention is to provide a method for identifying rhizoma dryopteris crassirhizomae, which comprises the following steps: (1) Preparation of a control solution: Taking a proper amount of trans-nerolidol reference substance, precisely weighing, and adding ethyl acetate to prepare a solution containing 0.09 mg in