Standard chemical fingerprint acquisition device for traditional Chinese medicinal materials

Abstract

The utility model belongs to the technical field of chromatographic analysis, and discloses a traditional Chinese medicinal material standard chemical fingerprint acquisition device which comprises a bin body, the bin body is connected with a fastener, the fastener is provided with a front guide pipe and a rear guide pipe in a penetrating manner, the front guide pipe is communicated with a front shunting sieve plate, and the rear guide pipe is communicated with a rear sieve plate. According to the utility model, a sample background test is taken as a basic measurement background in advance, and an empty bin is simply standardized; and the sample bin is used as a physical standard reference device of a chemical fingerprint spectrum, so that an accessible, efficient and repeatable mode is provided for standardization of the fingerprint spectrum.

Description

Technical Field

[0001] The utility model relates to the technical field of chromatographic analysis, in particular to a device for obtaining standard chemical fingerprints of traditional Chinese medicines. Background Art

[0002] In the testing of samples from traditional Chinese medicine, grain, the environment, and agriculture, obtaining an overall chemical profile has long been a key focus of testing methods and evaluation research. Fingerprinting (chromatograms or spectra that reveal the chemical characteristics of DNA and proteins in tissues or cells, after appropriate processing and analytical methods) has gained widespread recognition and is being applied in a variety of areas, including quality control, traceability, authenticity verification, and grade evaluation, targeting raw materials, finished products, and in-process products.

[0003] Fingerprints for traditional Chinese medicines were first proposed in this century and have been widely introduced into the quality analysis of injections, medicinal materials, preparations, and decoction pieces, with relevant specifications established in the pharmacopoeia. However, in current applications, establishing standardized fingerprints is difficult due to factors such as sample source, process interference, component diversity, complexity of preparation and extraction, and in-depth research on components. Furthermore, the reproducibility of testing batches of the same sample is poor, and the inter-batch variation of qualitative components, especially those with low content, is even greater. In many cases, it is difficult to form a basis for consistent evaluation of product quality, resulting in biased quality indicators in large-scale production and process control, which is not conducive to relevant quality assurance and accurate raw material identification.

[0004] Analysis of the chemical fingerprinting process revealed that one of the main reasons for poor reproducibility within a batch is the diversity of the source samples used to create the fingerprints, which contributes significantly to the overall uncertainty. Currently, research is underway to address the diversity of source sample preparation methods, with some standardized extraction methods proposed, particularly standardized and programmed extraction methods, to ensure a stable starting point for fingerprinting. For example, Chinese patent CN03157171.9 discloses an online extraction device and its application, which utilizes online extraction to rapidly prepare preliminary samples. However, this approach does not address the issues of selecting multiple sample types or standardizing the device. Utility Model Content

[0005] This utility model aims to provide a device for obtaining standard chemical fingerprints of traditional Chinese medicines. This device uses a sample background test as a basic measurement background to perform simple standardization of the empty chamber. The sample chamber serves as a physical standard reference device for chemical fingerprints, a quasi-metrological accessory for process and quality control, and provides an accessible, efficient, and repeatable method for fingerprint standardization. This device solves the problems mentioned in the previous art.

[0006] In order to achieve the above purpose, the present invention provides the following technical solutions:

[0007] A device for obtaining a standard chemical fingerprint of a traditional Chinese medicine comprises a chamber body, a sample column arranged on the inner side of the chamber body, and the outer diameter of the sample column is equal to the inner diameter of the chamber body; the liquid inlet and liquid outlet ends of the chamber body are respectively connected to a front conduit and a rear conduit for connecting to a liquid chromatography quantitative loop or an analytical flow path; the chamber body is detachably connected to a fastener, and the front conduit and the rear conduit are both passed through the fastener.

[0008] Furthermore, the front conduit is connected to a front diversion sieve plate on the inner side of the chamber body, the rear conduit is connected to a rear sieve plate on the inner side of the chamber body, and both ends of the sample column are respectively in contact with the front diversion sieve plate and the rear sieve plate.

[0009] The beneficial effects of the technical solution are:

[0010] This utility model proposes methods such as pre-sample background testing as a basic measurement background and simple standardization with an empty chamber, using the sample chamber as a physical standard reference device for chemical fingerprints and a quasi-metering accessory for process and quality control. Unlike simple online extraction, the fingerprint is used as a reference for identification and component analysis, not just a standard substance or sample in the conventional sense, thus changing the understanding of standard reference materials. This utility model implements a physical standardization device for obtaining fingerprints of samples such as Chinese medicinal materials, establishes efficient and repeatable sample reference quality indicators for quality control and method standardization, and can be applied to chemical quality and material profile analysis in traditional Chinese medicine, grain and oil, food, agriculture, environment, and life sciences. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 This is a cross-sectional view of a device for obtaining a standard chemical fingerprint of a Chinese medicinal material according to the present invention;

[0012] Figure 2 The utility model is a structural schematic diagram of a device for obtaining standard chemical fingerprints of traditional Chinese medicine.

[0013] The names of the corresponding symbols in the accompanying drawings are:

[0014] Chamber body 1, fastener 2, front conduit 3, front splitter sieve plate 4, rear sieve plate 6, sample column 5, rear conduit 7. DETAILED DESCRIPTION

[0015] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments:

[0016] like Figure 1 and Figure 2As shown, a device for obtaining a standard chemical fingerprint of a traditional Chinese medicine comprises a bin body 1, a sample column 5 is arranged on the inner side of the bin body 1, and the outer diameter of the sample column 5 is equal to the inner diameter of the bin body 1; the liquid inlet end and the liquid outlet end of the bin body 1 are respectively connected with a front conduit 3 and a rear conduit 7 for connecting to a liquid chromatography quantitative loop or an analysis flow path, the front conduit 3 is connected with a front diversion sieve plate 4 on the inner side of the bin body 1, and the rear conduit 7 is connected with a rear sieve plate 6 on the inner side of the bin body 1, and the two ends of the sample column 5 are respectively abutted against the front diversion sieve plate 4 and the rear sieve plate 6; the two ends of the bin body 1 are connected with fasteners 2 by threads, and the front conduit 3 and the rear conduit 7 are both passed through the fasteners 2.

[0017] Example 1

[0018] Dried ginseng was selected as a sample. After a typical sample was taken, it was crushed using a small ball mill. The sample powder was sieved and a granular powder of 70-75 μm was selected as a sample. The sample was examined under a microscope and found to be in a columnar powder sample with a uniform appearance. The sample was subjected to fingerprint determination. Liquid phase ultraviolet was used and acetonitrile water was used as the mobile phase for gradient elution. A total of 14 main peaks were obtained. The peak responses were all greater than 10% of the response under the 100% measurement scale of the vertical axis. Three substances including Rg1 were quantitatively determined and the relative normalized peak area values ​​of the 14 peaks were recorded. The sample was filled to form a small column and pressed into the front of the chamber body 1. , the back pressure and dead volume tests of the chamber body 1 were repeated multiple times, respectively, at 5 psi and 0.5 minute fluid volume (at a flow rate of 1 mL / min). After the small column was loaded into the chamber, it was connected to the liquid chromatography quantitative loop part, and the injection measurement was performed according to the normal liquid chromatography operation method, wherein the injection volume was set to 200 μL (according to the column size design, 1.2 g of powder was filled, and the small column in this embodiment was 0.2 cm × 0.5 cm). The back pressure of the small column was about 62 psi, and the deviation of six repetitions was less than 1%. The effluent detection volume was set at 2 mL, and the UV spectrum similarity deviation was less than 2%, and the concentration deviation was less than 1%. The overall sample test results are shown in Table 1:

[0019] Table 1 Dry ginseng sample test table

[0020]

[0021]

[0022] The samples of raw powder were processed according to the conventional fingerprint method. The main deviation came from the preparation of the samples, showing obvious extraction deviation at different content stages. The quantitative results of three substances such as Rg1 had the same trend as the above relative value comparison. The extraction integrity of the small column was 5% higher than that of the raw powder group.

[0023] Example 2

[0024] Roasted coffee beans were selected as samples. After the typical samples were taken, they were crushed using a small ball mill. The sample powder was sieved and 50-60 μm particle powder was selected as the sample. The sample was examined under a microscope and found to be generally round and amorphous powder sample with uniform appearance. During the filling process of the small column, it was found that its column formation was poor. Therefore, C18 filler with a mixed particle size of 50 μm was filled into a column. The fingerprint spectrum of the sample was determined. Liquid phase UV was also used, and acetonitrile water was used as the mobile phase for gradient elution. A total of 8 main peaks were obtained. The peak response was greater than 10% under the measurement scale of 100% on the vertical axis. The relative normalized peak area values ​​of the 8 peaks were recorded. The sample was then Filling, forming a small column, before being pressed into the chamber body 1, the chamber body 1 is subjected to back pressure and dead volume tests, which are repeated multiple times, respectively, at 3 psi and 0.4 minute fluid volume (at a flow rate of 1 mL / min). After the small column is pressed into the chamber, it is connected to the liquid chromatography quantitative loop part, and the injection measurement is performed according to the normal liquid chromatography operation method, wherein the injection volume is set to 300 μL (according to the column size design, 1.7 g of powder is filled, and the small column in this embodiment is 0.2 cm × 0.5 cm), the back pressure of the small column is about 73 psi, the six repetitions The deviation is less than 1%, the effluent detection volume is set at 2 mL, the UV spectrum similarity deviation is less than 2%, and the concentration deviation is less than 1%. The overall sample test results are shown in Table 2:

[0025] Table 2 Coffee bean sample test table

[0026]

[0027] The raw powder samples were prepared according to the conventional fingerprint method, and the main deviation came from the sample preparation, showing obvious extraction deviations at different content stages.

[0028] Example 3

[0029] The ethanol extract of Panax ginseng semi-fluid was selected as the sample and mixed with 100 μm C18 filler. The sample was fingerprinted using liquid phase UV with acetonitrile and water as the mobile phase for gradient elution. A total of 12 major peaks were obtained. The peak response was greater than 10% on the vertical axis (100%). The relative normalized peak area values ​​of the 12 peaks were recorded.

[0030] The sample was then loaded to form a small column. Before being loaded into the chamber body 1, the chamber body 1 was subjected to back pressure and dead volume tests, which were repeated multiple times, with the values ​​being 4 psi and 0.5 minute fluid volume (at a flow rate of 1 mL / min). After the small column was loaded into the chamber, it was connected to the liquid chromatography quantitative loop portion and injection was performed according to normal liquid chromatography operation. The injection volume was set to 200 μL (designed according to the column size, 1.3 g of powder was loaded, and the small column in this embodiment was 0.2 cm × 0.5 cm). The back pressure of the small column was approximately 61 psi. The deviation of the six repetitions was less than 1%. The effluent detection volume was set at 2 mL. The UV spectrum similarity deviation was less than 2%, and the concentration deviation was less than 1%. The overall sample test results are shown in Table 3:

[0031] Table 3 Test table of ethanol extract samples of ginseng semi-fluid

[0032]

[0033] The above description is merely an embodiment of the present invention, and the commonly known specific technical solutions or features in the solution are not described in detail here. It should be noted that for those skilled in the art, without departing from the technical solution of the present invention, several variations and improvements can be made, which should also be considered as the scope of protection of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection claimed in this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.

Claims

1. A device for obtaining standard chemical fingerprints of Chinese medicinal materials, characterized in that: It includes a chamber body, a sample column is arranged on the inner side of the chamber body, and the outer diameter of the sample column is equal to the inner diameter of the chamber body; the liquid inlet end and the liquid outlet end of the chamber body are respectively connected to a front tube and a rear tube for connecting to a liquid chromatography quantitative loop or an analytical flow path, and the chamber body is detachably connected to a fastener, and the front tube and the rear tube are both passed through the fastener.

2. The device for obtaining a standard chemical fingerprint of a Chinese herbal medicine according to claim 1, characterized in that: The front conduit is connected to a front shunt sieve plate on the inner side of the chamber body, the rear conduit is connected to a rear sieve plate on the inner side of the chamber body, and both ends of the sample column are respectively in contact with the front shunt sieve plate and the rear sieve plate.

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