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Method for detecting content of compounds in Huoxiang Zhengqi oral liquid by liquid chromatography-mass spectrometry

A technology of Zhengqi Oral Liquid and liquid chromatography, which is applied in the field of pharmaceutical component analysis, can solve the problems of low active ingredients and inability to accurately detect the content of Huoxiang Zhengqi Oral Liquid, and achieve good separation, repeatability and precision.

Pending Publication Date: 2022-03-18
TAIJI GRP CHONGQING FULING PHARM FACTORY CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In short, the existing technology cannot accurately detect the content of index components in Huoxiang Zhengqi Oral Liquid, especially the active ingredients with relatively low content

Method used

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  • Method for detecting content of compounds in Huoxiang Zhengqi oral liquid by liquid chromatography-mass spectrometry
  • Method for detecting content of compounds in Huoxiang Zhengqi oral liquid by liquid chromatography-mass spectrometry
  • Method for detecting content of compounds in Huoxiang Zhengqi oral liquid by liquid chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1UHPLC / Q-Orbitrap MS detection condition verification

[0054] Liquid phase conditions: Waters ACQUITY BEH Shield RP18 (1.7μm, 2.1×100mm) chromatographic column, with 0.1% formic acid aqueous solution (A)-0.1% formic acid acetonitrile (B) as mobile phase, column temperature 35°C, flow rate 0.2mL / min, and the injection volume was 1 μL. The elution gradient is shown in Table 1.

[0055] Table 1 Mobile phase elution gradient

[0056] time / min Acetonitrile (B) 0.1% formic acid water (A) 0-1 5-10 95-90 1-12 10-20 90-80 12-20 20-27 80-73 20-24 27-33 73-67 24-30 33-40 67-60 30-33 40-48 60-52 33-42 48-80 52-20 42-42.5 80-95 20-5 42.5-45 95 5

[0057] Mass Spectrometry Condition Optimization

[0058] As the energy of NCE increases, the kurtosis of precursor ion fragments gradually decreases, while the kurtosis of characteristic product ion fragments gradually increases. If the energy is too hi...

Embodiment 2

[0063] Embodiment 2 specificity verification

[0064] Specificity refers to the ability of the method to accurately detect the characteristics of the target compound in the presence of other components (impurities, excipients) that may exist. Under the chromatographic and mass spectrometric conditions in Example 1, the blank solvent, mixed standard solution, and Huoxiangzhengqi oral liquid samples were injected respectively, and the results in the positive and negative ion scanning modes were as follows: Figure 1-3 As shown, the results showed that nine target compounds and internal standards could be accurately detected without any interference, which indicated that the method had high selectivity.

Embodiment 3

[0065] Implement 3 linear range, LODs and LOQs verification

[0066] Using a series of concentration prepared mixed standard solutions, by plotting the peak area (A sample / A IS ) relative to each analyte concentration (C sample / C IS ) to create a standard curve. Then perform linear regression on the standard curve, and view the correlation coefficient and linear range of the resulting linear regression equation. The correlation coefficient should satisfy r 2 ≥0.999, the concentration of all samples should be located between the highest and lowest concentration of the standard curve as much as possible. The results are shown in Table 3, the linear regression equations of 9 target compounds were obtained, the correlation coefficient was good, r 2 The average is 0.999.

[0067] Table 3 The linear range of 9 compounds

[0068]

[0069] Further, the limit of detection and the limit of quantitation were measured with a signal-to-noise ratio (S / N) of 3 and 10, and the re...

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Abstract

The invention belongs to the technical field of pharmaceutical component analysis, and particularly relates to a method for detecting the content of compounds in Huoxiang Zhengqi oral liquid through liquid chromatography-mass spectrometry. The method comprises the following steps: carrying out gradient elution separation by using liquid chromatography, and then carrying out mass spectrometric detection, in the detection process, liquiritin, glycyrrhizic acid, hesperidin, naringin, magnolol, honokiol and pachymic acid A are detected in a negative ion scanning mode; detection in a positive ion scanning mode shows that the corresponding NCE energy of liquiritin is 50 V, the corresponding NCE energy of glycyrrhizic acid is 30 V, the corresponding NCE energy of hesperidin is 50 V, the corresponding NCE energy of naringin is 30 V, the corresponding NCE energy of magnolol is 70 V, the corresponding NCE energy of honokiol is 70 V, the corresponding NCE energy of pachymic acid A is 50 V, the corresponding NCE energy of water and oxidized peucedanin is 50 V, and the corresponding NCE energy of nobiletin is 50 V. The detection method is good in repeatability and precision, and can be used for qualitatively and quantitatively detecting hydrated oxypeucedanin and nobiletin with relatively low contents in the hydrated oxypeucedanin and nobiletin.

Description

technical field [0001] The invention belongs to the technical field of medicament component analysis, and in particular relates to a method for detecting compound content in Huoxiangzhengqi oral liquid by liquid chromatography-mass spectrometry. Background technique [0002] Huoxiang Zhengqi Oral Liquid, the name of Chinese patent medicine. It is a heat-dispelling agent, which has the effects of relieving exterior and removing dampness, regulating qi and harmonizing the middle. It is used for cold caused by exogenous wind-cold, internal injury damp stagnation or summer injury and summer dampness. Symptoms include headache, dizziness, fullness of chest and diaphragm, abdominal pain, vomiting and diarrhea; stomach-type cold. Huoxiang Zhengqi Oral Liquid is recorded in the 2020 edition of "Chinese Pharmacopoeia", which records the determination of the content of hesperidin, honokiol and the total content of magnolol by different HPLC methods. In order to improve and perfect t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/86
CPCG01N30/02G01N30/72G01N30/8679Y02A50/30
Inventor 余河水董自亮彭涛李正刘世琪吴梦凡原欢欢禹奇男
Owner TAIJI GRP CHONGQING FULING PHARM FACTORY CO LTD
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