Method for identifying six components in tendon-relaxing and blood-activating pills by UPLC-Q-TOF method

A technology of blood pills and formic acid, applied in the field of chemical analysis, can solve the problems of long analysis time and complicated extraction process, and achieve the effect of promoting effective extraction, simple method and high-quality chromatographic peak shape.

Pending Publication Date: 2022-07-15
CHONGQING INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Shujinhuoxue Pills contain Dipsacus saponin Ⅵ, β-ecdysterone, naringin, amygdalin, catechin and (±) prohematoxylin B and other components. The qualitative identification of Guizhi, Panax notoginseng, Angelica dahurica and Radix Paeoniae Rubra in this preparation is complicated and takes a long time for analysis, and does not involve the qualitative identification of Dipsacus, Achyranthes bidentata, Drynaria rhizome, peach kernel, catechin and sumac identify

Method used

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  • Method for identifying six components in tendon-relaxing and blood-activating pills by UPLC-Q-TOF method
  • Method for identifying six components in tendon-relaxing and blood-activating pills by UPLC-Q-TOF method
  • Method for identifying six components in tendon-relaxing and blood-activating pills by UPLC-Q-TOF method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Sample pretreatment

[0045] 1) Prepare the test solution: 1 pill of Shujin Huoxue Pills, cut into pieces, add 5 g of diatomaceous earth, mix well and grind, then add 50 mL of anhydrous ethanol, ultrasonically treat for 20 min, filter, take 0.2 mL of the filtrate, add methanol The solution was diluted to 10 mL, shaken well, and filtered with a microporous membrane (0.22 μm), and the subsequent filtrate obtained was the test solution.

[0046] 2) Prepare the reference substance solution: take appropriate amounts of the reference substances of saponin VI, β-ecdysterone, naringin, amygdalin, catechin, ± protohematoxylin B respectively, accurately weigh them, and add methanol solution to prepare them respectively. A solution with a content of 2 μg / mL was obtained, and then filtered through a microporous membrane (0.22 μm), and the obtained subsequent filtrate was the reference solution.

[0047]3) Configure the negative reference solution: respectively according ...

Embodiment 2

[0049] Example 2 Screening of mobile phase

[0050] The chromatographic behavior and ionization degree of 6 compounds in the mobile phase of acetonitrile and different kinds of volatile buffers (0.1% formic acid, 0.02 mmol / L ammonium formate solution, 0.02 mmol / L ammonium formate solution containing 0.1% formic acid) were investigated impact, as follows:

[0051] 1. Chromatographic conditions

[0052] Chromatographic column: Waters ACQUITY UPLC BEH C18 (50×2.1 mm, 1.7 μm) chromatographic column; the column temperature is 30° C., the injection volume is 1 μL, and the volume flow rate is 0.3 mL / min.

[0053] ① Mobile phase A contains 0.1% formic acid in 0.02 mmol / L ammonium formate solution; mobile phase B contains 0.1% formic acid in acetonitrile.

[0054] ②Gradient elution 0~4min, mobile phase A90%-50%, mobile phase B10%-50%.

[0055] 2. Mass Spectrometry Conditions

[0056] Electrospray ionization negative ion mode; mass scanning range: 100~1000m / z; Q-TOF full scan (MS); ...

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Abstract

The invention belongs to the technical field of chemical analysis, and particularly relates to a method for identifying six components in a tendon-relaxing and blood-activating pill by a UPLC-Q-TOF (Ultra Performance Liquid Chromatography-Quantitative Time of Flight) method, and the six components comprise dipsacus asper saponin VI, beta-ecdysterone, naringin, amygdalin, catechin and + / -protosappanin B. According to the method, a Waters ultra-high-speed liquid chromatograph and a small-particle-size chromatographic column special for an ultra-high-speed liquid phase instrument are adopted for gradient elution, a mobile phase A is a mixed solution of ammonium formate and formic acid, the concentration of ammonium formate is 0.02 mmol / L, the volume concentration of formic acid is 0.1%, a mobile phase B is a mixed solution of formic acid and acetonitrile, and the volume concentration of formic acid is 0.1%; a detection instrument is a quadrupole time-of-flight tandem mass spectrum, and a scanning mode is an electrospray ionization anion mode. According to the method established by the invention, the six components in the tendon-relaxing and blood-activating pill can be accurately identified, whether the pill contains teasel root, achyranthes bidentata, rhizoma drynariae, peach kernel, catechu and sappan wood or not can be judged, and the method has important significance for comprehensively evaluating the quality of the tendon-relaxing and blood-activating pill.

Description

technical field [0001] The invention belongs to the field of chemical analysis, and specifically relates to a method for identifying 6 components in Shujin Huoxue Pills by UPLC-Q-TOF method. Background technique [0002] Shujin Huoxue Pill is composed of continuum, Achyranthes, Rhizoma Drynariae, peach kernel, catechu, hematoxylin, soil soft-shelled turtle, safflower, Rehmannia glutinosa, Angelica dahurica, gardenia, red peony root, cinnamon twig, Panax notoginseng, frankincense (made ), natural copper (vinegar calcined), rhubarb, strychnine, angelica and borneol composed of dark brown honey pills. The medicine is bitter and astringent in taste, has the functions of relaxing tendons and dredging collaterals, promoting blood circulation and relieving pain, and can be used for bruises, waist and qi, broken tendons and fractures, and pain caused by blood stasis. [0003] Shujin Huoxue Pills include Chuanxudan saponin VI, β-ecdysterone, naringin, amygdalin, catechin, and (±) pr...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/26G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/26G01N30/72G01N30/8631G01N2030/027G01N2030/062
Inventor苏晶汪杨丽李青白小琼陈晓虎王慧唐华葛渊源张毅蒋万浪
OwnerCHONGQING INST FOR FOOD & DRUG CONTROL