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A kind of detection method of stagnation-dispelling analgesic drug

A technology for analgesia and detection methods for Sanjie, which can be applied to measurement devices, instruments, scientific instruments, etc., and can solve the problems of labor-consuming reagents, complicated pretreatment process of detection methods, and small quantities.

Active Publication Date: 2019-03-19
JIANGSU KANION PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these quality control methods disclosed in the prior art need to classify the ingredients in the stagnation-dissolving analgesic drugs by different methods, and then measure them separately or by classification, resulting in a single type of ingredients that can be detected simultaneously at one time, and often the quantity is relatively large. The purpose of quickly and efficiently evaluating the quality of drugs cannot be achieved; in addition, the pretreatment process of existing detection methods is usually complicated, and consumes a lot of reagents and manpower

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  • A kind of detection method of stagnation-dispelling analgesic drug
  • A kind of detection method of stagnation-dispelling analgesic drug
  • A kind of detection method of stagnation-dispelling analgesic drug

Examples

Experimental program
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Effect test

Embodiment 1

[0080] Chromatographic conditions:

[0081] Chromatographic column Agilent Zorbax SB-C18 (column length is 100mm, inner diameter is 3.0mm, particle size is 1.8μm); mobile phase is acetonitrile (A)-0.1% formic acid aqueous solution (B) gradient elution, linear elution program as shown in the table 1; flow rate: 0.4ml min-1; column temperature: 30°C; injection volume: 3μL.

[0082] Table 1: Gradient elution program of Example 1

[0083]

[0084]

[0085] Mass Spectrometry Conditions:

[0086] Using ESI source, 0~12.6min, positive ion mode, 12.6~50min, negative ion mode; capillary voltage 4000V, atomizing gas pressure 45psi, drying gas flow rate 10L / min, heating capillary temperature 350℃, source debris voltage: 210V, Skimmer 65V, mass scanning range m / z 100~2500.

[0087] Table 2 shows the extracted ion information of 14 main compound components and 3 selected internal standards in the mass-dissolving and analgesic drugs detected by the present invention for integral ca...

Embodiment 2

[0105] Adopt the same technical scheme of embodiment 1 to detect the fingerprint of the need testing solution that obtains, and calculate the chromatographic peak according to the fingerprint that obtains, and calculate the content of 14 kinds of main components in the need testing according to standard curve; In this embodiment, the ultrasonic extraction method is used to replace the reflux extraction method in Example 1. The ultrasonic extraction method in this embodiment is ultrasonic extraction (250W, 40KHz) for 1h.

[0106] Test results such as Figure 4 as shown, Figure 4 It is the fingerprint of the solution to be tested obtained in Example 2 of the present invention.

Embodiment 3

[0108] Adopt the same technical scheme of embodiment 1 to detect the fingerprint of the need testing solution that obtains, and calculate the chromatographic peak according to the fingerprint that obtains, and calculate the content of 14 kinds of main components in the need testing according to standard curve; In this embodiment, the vortex extraction method is used to replace the reflux extraction method in Example 1. The vortex extraction method in this embodiment is to vortex on a vortex mixer for 10 minutes.

[0109] Test results such as Figure 5 and as shown in Table 4, Figure 5 It is the fingerprint of the test solution obtained in Example 3 of the present invention, and Table 4 is the content of main components in the test solution obtained in Examples 1 to 3 of the present invention.

[0110] Table 4 Examples 1-3 use three kinds of extraction methods to measure the content of each component of the test product (mg / g) respectively

[0111]

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Abstract

A method for detecting a stasis-removing pain-relieving medicine is disclosed. The method includes 1) mixing the stasis-removing pain-relieving medicine with a solvent, and performing extraction to obtain a solution of a test product; 2) detecting the solution of the test product by liquid chromatography-mass spectrometry to obtain a fingerprint; and 3) according to the fingerprint, a standard curve and the mass of the test product of the medicine, acquiring contents of fourteen components in the test product. A UPLC / Q-TOF MS manner is adopted in the method, and negative-positive ion full-scanning mode is adopted, and therefore a plurality of compounds can be effectively distinguished, components of the medicine are qualitatively and quantitatively detected, and the components of fourteen different types in the medicine can be detected. The method has characteristics of simple sample treatment operation, a low sample using amount, high precision, capability of being accurate and rapid, high stability, good repeatability and a high recovery rate, and can be adopted as an effective detecting method at present for comprehensively controlling quality of the stasis-removing pain-relieving medicine.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to a detection method for stagnation-dissolving and analgesic drugs. Background technique [0002] The analgesic medicine for dispelling stagnation is a prescription preparation composed of Panax notoginseng, dragon's blood jellyfish, fritillary fritillary and coix seed. Secondary dysmenorrhea, irregular menstruation, pelvic mass, infertility, endometriosis and other diseases have a good curative effect on endometriosis in clinical use. The main components of stagnation-relieving and analgesic drugs are saponins, phenolic acids, alkaloids and oils, etc. These ingredients are crucial to the efficacy of stagnation-relieving and analgesic drugs. In order to better control the quality of medicines and ensure the clinical efficacy of medicines, it has become a research hotspot in this field to detect the related components of stagnation-relieving and analgesic medicines and to establish a m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 萧伟秦建平潘有智林夏李家春黄文哲王振中
Owner JIANGSU KANION PHARMA CO LTD
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