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Method for determining content of six aristolochic acid components in asarum

A method of determination, the technology of aristolochic acid, applied in the field of traditional Chinese medicine, can solve the problem of no related reports of asarum, and achieve a highly specific effect

Active Publication Date: 2021-08-13
HEBEI INST FOR DRUG & MEDICAL DEVICE CONTROL (HEBEI INST FOR COSMETICS CONTROL)
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] There have been many research reports on the analytical methods for the determination of aristolochic acids in medicinal materials, mainly using reversed-phase high-performance liquid chromatography (RPLC) and high-performance liquid phase tandem mass spectrometry (HPLC-MS), but the highest rate of medicinal Asarum has no relevant reports, and mainly focuses on individual components such as aristolochic acid I and II

Method used

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  • Method for determining content of six aristolochic acid components in asarum
  • Method for determining content of six aristolochic acid components in asarum
  • Method for determining content of six aristolochic acid components in asarum

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] instrument

[0050] Waters Acquity UPLC / XEVO TQ-S ultra-high performance liquid chromatography-triple quadrupole mass spectrometer; KQ-400KDE ultrasonic cleaning instrument (Kunshan Ultrasonic Instrument Co., Ltd.); AE240 electronic balance (Shanghai Mettler Instrument Co., Ltd. );

[0051] Reagent

[0052] Reference substance: aristolochic acid A (Shanghai Shidande, batch number: 3114, content 98.0%), aristolochic acid B (Shanghai Shidande, batch number: 3519, content 99.7%), aristolochic acid C (Shanghai Shidande, batch number: 3519, content 99.7%), aristolochic acid C (Shanghai Shidande Shidande, batch number: 4328, content 95.1%), aristolochic acid D (Shanghai Shidande, batch number: 4327, content 94.5%), aristolochic acid Ⅲ (Shanghai Shidande, batch number: 3520, content 99.4%) %), aristolochic acid Ⅶa (Shanghai Dande, batch number: 3521, content 99.6%),

[0053] Methanol, acetonitrile, formic acid (chromatographically pure, Merck Company); water is deionized wa...

Embodiment 2

[0084] Chromatographic conditions: Chromatographic column: Water C 18 Column (1.7μm, 2.1×50mm); Acetonitrile is used as mobile phase A, 0.2% formic acid is used as mobile phase B, gradient elution program is shown in Table 1; column temperature: 30°C, flow rate: 0.3ml·min -1 .

[0085] Mass spectrometry conditions: ion source: ESI, scan mode: positive ion scan, monitoring mode: multiple reaction monitoring mode (MRM), capillary voltage: 3.00kV, cone voltage: 60V, desolvation temperature: 350°C, see mass spectrometry parameters for details Table 2.

[0086] Preparation of mixed reference substance solution: Take appropriate amount of aristolochic acid A, B, C, D, III and Ⅶa reference substances, weigh them accurately, add methanol to make a mixed reference substance solution containing 50ng per 1ml, and get ready.

[0087] Preparation of the test solution: take Asarum decoction pieces, pulverize (pass through a No. 4 sieve), get about 0.5g, accurately weigh, put in a stoppere...

Embodiment 3

[0090] Chromatographic conditions: Chromatographic column: Water C 18 Column (1.7μm, 2.1×50mm); acetonitrile as mobile phase A, 0.1% formic acid as mobile phase B, gradient elution program as shown in Table 1; column temperature: 30°C, flow rate: 0.3ml min -1 .

[0091] Mass spectrometry conditions: ion source: ESI, scan mode: positive ion scan, monitoring mode: multiple reaction monitoring mode (MRM), capillary voltage: 3.00kV, cone voltage: 60V, desolvation temperature: 350°C, see mass spectrometry parameters for details Table 2.

[0092] Preparation of mixed reference substance solution: Take appropriate amount of aristolochic acid A, B, C, D, III and VIIa reference substances, weigh them accurately, add methanol to make a mixed reference substance solution containing 10 ng per 1 ml, and get ready.

[0093] Preparation of the test solution: take Asarum decoction pieces, pulverize (pass through a No. 4 sieve), get about 0.5g, accurately weigh, put in a stoppered Erlenmeyer...

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Abstract

The invention discloses a method for determining the content of six aristolochic acid components in asarum, and belongs to the technical field of traditional Chinese medicine, a UPLC-MS / MS method is adopted for simultaneously determining the content of aristolochic acid A, aristolochic acid B, aristolochic acid C, aristolochic acid D, aristolochic acid III and aristolochic acid VIIa in asarum, the specificity is higher, more components are controlled, different medicinal parts are comprehensively measured and analyzed, so that the quality of the medicinal material is more comprehensively evaluated, and a basis is provided for reasonable application of the asarum medicinal material.

Description

technical field [0001] The present invention relates to a method for determining the content of six aristolochic acid components in Herba Asarum, specifically, to a method for simultaneously determining Aristolochic Acid A, Aristolochic Acid B, Aristolochic Acid C, Aristolochic Acid C, The invention discloses a method for determining the contents of six components of aristolochic acid D, aristolochic acid III and aristolochic acid VIIa, and belongs to the technical field of traditional Chinese medicines. Background technique [0002] Aristolochic acid (AA) is a nitrophenanthrene compound mainly found in Aristolochia plants. Due to the strong carcinogenicity of aristolochic acid, since 2003, my country's drug regulatory authorities have successively canceled the quality standards for medicinal materials such as Aokita, Guanmutong, Fangji, Tianxianteng, Aristolochia, etc., "Chinese Pharmacopoeia" 2020 edition one Only asarum is included in the book. Asarum is the dried roots ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/047Y02A50/30
Inventor 刘永利孙慧珠王晓蕾王常顺
Owner HEBEI INST FOR DRUG & MEDICAL DEVICE CONTROL (HEBEI INST FOR COSMETICS CONTROL)
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