Method for detecting aristolochic acid I content in Zhuifengtougu capsules based on UPLC method and sample pretreatment method

A technology for sample pretreatment and aristolochic acid, applied in the field of analytical chemistry, can solve the problems of sample emulsification, waste of time and resources, and inability of samples to enter the detection link, etc., to prevent emulsification, accurate detection, and ensure clinical drug safety. Effect

Pending Publication Date: 2020-09-11
HINYE PHARM CO LTD
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Problems solved by technology

However, this method is prone to sample emulsification in the process of alkali adjustment extraction and sample p...

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  • Method for detecting aristolochic acid I content in Zhuifengtougu capsules based on UPLC method and sample pretreatment method
  • Method for detecting aristolochic acid I content in Zhuifengtougu capsules based on UPLC method and sample pretreatment method
  • Method for detecting aristolochic acid I content in Zhuifengtougu capsules based on UPLC method and sample pretreatment method

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Embodiment 1

[0035] A method for detecting the content of aristolochic acid I in Zhuifeng Tougu capsules based on UPLC, comprising the following steps:

[0036] Step 1: Prepare the reference solution:

[0037] (1) Preparation of reference substance stock solution

[0038] Take about 10mg of aristolochic acid Ⅰ reference substance, weigh it accurately, put it in a 100mL measuring bottle, add methanol to dissolve and dilute to the mark, and the concentration is about 100μg / mL;

[0039] (2) Preparation of reference substance mother liquor

[0040] Accurately measure 5.0 mL of the stock solution of aristolochic acid reference substance in a 100 mL measuring bottle, add methanol to dilute to the mark, and the concentration is about 5 μg / ml;

[0041] (3) Preparation of reference substance

[0042] Precisely measure 5.0ml of aristolochic acid Ⅰ reference substance mother solution in a 50ml measuring bottle, add methanol to dilute to the mark, and the concentration is about 0.5μg / mL;

[0043] ...

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Abstract

The invention discloses a method for detecting aristolochic acid I content in Zhuifengtougu capsules based on a UPLC method and a sample pretreatment method. According to the method, a Zhuifengtougu capsule sample is pretreated in a manner of combining liquid-liquid extraction and solid-phase extraction, wherein liquid-liquid extraction is acid regulation extraction, so that not only can an emulsification phenomenon be effectively prevented from occurring in a sample preparation process, but also a solid-phase extraction small column can be effectively prevented from being blocked by sample loading liquid, meanwhile, the recovery rate of aristolochic acid I is guaranteed, and a very good impurity removal effect is achieved. According to the invention, the content of aristolochic acid I inthe Zhuifengtougu capsules is further analyzed in combination with UPLC, specific pretreatment and chromatographic detection conditions are adopted, the aristolochic acid I can be effectively separated in the liquid chromatography, the separation degree reaches 1.5 or above, the impurity interference is extremely small, the content of the aristolochic acid I in the Zhuifengtougu capsules can be effectively, simply, conveniently and accurately detected, and then the safety and stability of clinical medication of the Zhuifengtougu capsules are ensured.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, and more specifically, to a method for detecting the content of aristolochic acid I in Zhuifeng Tougu capsules based on UPLC method and a sample pretreatment method. Background technique [0002] Zhuifeng Tougu Capsule is a variety listed in the standards of the State Food and Drug Administration. Composed of twenty-four traditional Chinese medicines such as Chuanwu, Asarum, and Dilong, it has the effects of dredging the meridian, dispelling rheumatism, relieving pain and dispelling cold, and is used for anemofrigid-damp arthralgia, arthralgia in limbs, numbness of hands and feet, etc. Among them, asarum contains aristolochic acid Ⅰ, a component of chronic kidney damage, and long-term use can lead to late renal failure. Therefore, the limited detection of aristolochic acid Ⅰ in Zhuifeng Tougu capsule is of great significance to control the quality of the product preparation and ensu...

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Application Information

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IPC IPC(8): G01N30/06G01N30/02
CPCG01N30/02G01N30/06G01N2030/062
Inventor 余彬彬马洁高玉贺丁扬洲何一刘波李亚慧
Owner HINYE PHARM CO LTD
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