Method for determination of illegally added substances in traditional Chinese medicines and health-care products

A technology of illegally added and health care products, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of endangering the health of consumers, affecting the reputation of traditional Chinese medicine and health food, etc., to avoid false positive results, save time, and operate The effect of simple method

Inactive Publication Date: 2015-10-21
SHANDONG ANALYSIS & TEST CENT
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  • Description
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Problems solved by technology

In recent years, driven by profit, some unscrupulous manufacturers have taken advantage of people's belief that traditional Chinese medicine and health care products are pure natural non-toxic by-products and can be taken for a long time to illegally add various antihypertensive and hypoglycemic chemical drugs to traditional Chinese medicine preparations or health foods. Not only seriously affected the reputation of traditional Chinese medicine and health food, but also endangered the health of consumers

Method used

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  • Method for determination of illegally added substances in traditional Chinese medicines and health-care products
  • Method for determination of illegally added substances in traditional Chinese medicines and health-care products
  • Method for determination of illegally added substances in traditional Chinese medicines and health-care products

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Experimental program
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Effect test

Embodiment 1

[0072] Optimization of mass detection conditions

[0073] The declustering voltage (DP) and collision energy (CE) of 13 chemical drugs were optimized to maximize the transmission efficiency of the sample precursor ions and the higher response intensity of the product ions in the mass spectrum, thereby improving the sensitivity of the detection method.

[0074] The experimental method is as follows: First, in the selected ion detection mode, input the mass-to-charge ratio of the sample precursor ions, optimize the declustering voltage (0V~300V), and ensure the maximum transmission efficiency of the precursor ions, that is, reach the collision cell as much as possible; In the product ion scan mode, investigate the influence of different collision energy on the peak intensity of the parent ion and the product ion, and select the collision energy when the parent ion almost disappears and the product ion intensity is the largest. After optimization, the optimal declustering voltage and ...

Embodiment 2

[0079] A method that can simultaneously qualitatively and quantitatively detect 13 kinds of antihypertensive or antihypertensive chemical drugs illegally added to Chinese medicines and health products, including the following:

[0080] 1. HPLC-MS / MS Coupled Instrument

[0081] 1.1 HPLC conditions

[0082] Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6mm×50mm, 1.8μm, Agilent Technologies Co., Ltd.). Mobile phase: Phase A is an aqueous solution containing 0.1% formic acid (volume ratio), phase B is acetonitrile. Gradient elution procedure: 0~2min, phase B keeps 10%; 2~8min, phase B rises from 10% to 80%; 8~10min, phase B keeps 80%; 10.1min-15min, phase B drops to 10% ; Stop after 15min. Flow rate: 0.4 mL / min. Column temperature: 35°C, injection volume: 5.00μL.

[0083] 1.2 MRM quantitative detection conditions

[0084] Ion source: Electrospray ion source (+ESI), using positive ion mode for detection. Dry gas: N 2 , Collision gas: high-purity nitrogen. Curtain air pressure: 35....

Embodiment 3

[0106] Example 3 A health product testing example

[0107] Using the method of 1 and 2 in Example 2, weigh 0.20g of a health care product, and process it according to the pretreatment method of Example 2. The test solution is diluted 1000 times and then injected with 5μL for detection. The mass spectrometry results are as follows Figure 15 with Figure 16 (EPI spectrum) as shown. After testing, glibenclamide was illegally added to the sample, and the qualitatively tested EPI spectrum was consistent with the standard library. After calculation, the content of glibenclamide in the sample was 8.67 mg / g.

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Abstract

The invention discloses a method for determination of illegally added substances in traditional Chinese medicines and health-care products; with use of high performance liquid chromatography-tandem quadrupole linear ion trap mass spectrometry, the method which is capable of simultaneously qualitative and quantitative detection (multiple reaction monitoring sMRM-information dependent acquisition IDA-enhanced product ion scanning EPI detection) of 13 kinds of illegally added hypoglycemic hypotensive chemical drugs such as clonidine hydrochloride and gliclazide in the traditional Chinese medicines and the health-care products is developed. And through one-time sampling detection, not only can a quantitative result obtained, but also occurrence of a false positive result is effectively avoided through qualitative database screening. The establishment of the method provides a technical support for enacting detection standards of the illegally added hypoglycemic hypotensive chemical drugs in the traditional Chinese medicine and the health-care products.

Description

Technical field [0001] The invention belongs to the quality detection system of traditional Chinese medicine and health care, and specifically relates to a method for determining illegally added substances in traditional Chinese medicine and health care products. Background technique [0002] Hypertension and diabetes are common and frequently-occurring diseases, and their incidence is increasing rapidly with the improvement of people's living standards, changes in lifestyles, and aging of the age structure, which have seriously threatened human health. In recent years, driven by profits, some illegal manufacturers have taken advantage of people’s belief that Chinese medicines and health products are pure natural non-toxic by-products and can be taken for a long time, and illegally added various antihypertensive and hypoglycemic chemical drugs in Chinese medicine preparations or health foods. It not only seriously affected the reputation of Chinese medicine and health food, but a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 王珊珊赵汝松苑金鹏宁凡盛陈跃赵金
Owner SHANDONG ANALYSIS & TEST CENT
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