Detection method of accelerant M and accelerant DPG in Chinese patent medicine and healthcare food

A technology of health food and detection method, which is applied in the fields of mass spectrometry and drug chromatography, and can solve the problems of no screening and quantitative methods

Active Publication Date: 2019-07-30
苏州市药品检验检测研究中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There have been no reports of the addition of accelerator M and accelerator DPG, and there are no screening and quantitative methods for these two substances. In the long-term health food illegal addition test, our laboratory found that accelerator M alone or simultaneously with sildenafil Added to the product, the accelerator DPG was added to the product alone (see Table 1)

Method used

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  • Detection method of accelerant M and accelerant DPG in Chinese patent medicine and healthcare food
  • Detection method of accelerant M and accelerant DPG in Chinese patent medicine and healthcare food
  • Detection method of accelerant M and accelerant DPG in Chinese patent medicine and healthcare food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0104] A detection method for accelerator M in Chinese patent medicine and health food, comprising the following steps:

[0105] (1) Chromatographic conditions:

[0106] Chromatographic column: ACQUITY UPLC®HSS T3, 100mm×2.1mm, 1.8μm; detector: diode array detector; detection wavelength: 210nm; scanning wavelength range 190-400nm; mobile phase: A-0.1% formic acid solution, B-0.1 % formic acid-acetonitrile; flow rate: 0.3mL / min; column temperature: 30℃; injection volume: 1μL; elution gradient program: 0-2min, 10%B; 7-9min, 90%B; %B;

[0107] Mass Spectrometry Conditions:

[0108] Electrospray positive ion mode; Capillary voltage: 3500V; Drying gas flow rate: 10.0L / min; Atomizing gas pressure: 40psig; Drying gas temperature: 350°C; Fragmentation voltage: 135V; Mass spectrometry; acquisition mode: targetMS; precursor ion: 167.9934, retention time: 4.74min (chromatogram), 4.85min (mass spectrogram); collision energy: 25V, 35V; mass spectrometry scanning range: 50-1700;

[0109...

Embodiment 2

[0118] A detection method of accelerator DPG in Chinese patent medicine and health food, comprising the following steps:

[0119] (1) Chromatographic conditions:

[0120] Chromatographic column: ACQUITY UPLC®HSS T3, 100mm×2.1mm, 1.8μm; detector: diode array detector; detection wavelength: 205nm; scanning wavelength range 190-400nm; mobile phase: A-0.1% formic acid solution, B-0.1 % formic acid-acetonitrile; flow rate: 0.3mL / min; column temperature: 30℃; injection volume: 1μL; elution gradient program: 0-2min, 10%B; 7-9min, 90%B; %B;

[0121] Mass Spectrometry Conditions:

[0122] Electrospray positive ion mode; Capillary voltage: 3500V; Drying gas flow rate: 10.0L / min; Atomizing gas pressure: 40psig; Drying gas temperature: 350°C; Fragmentation voltage: 135V; Mass spectrometry; acquisition mode: targetMS; parent ion: 212.1197, retention time: 2.88min (chromatogram), 2.99min (mass spectrogram); collision energy: 15V, 30V; mass spectrometer scanning range: 50-1700;

[0123] ...

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Abstract

The invention provides a detection method of accelerant M and accelerant DPG in Chinese patent medicine and healthcare food. The detection method comprises the following steps: performing qualitativescreening and content determination by adopting an ultra-high-performance liquid chromatography-ultraviolet spectrum-flight time mass spectrograph, wherein a chromatographic condition is that the chromatographic column is C18 chromatographic column, a detector is a diode array detector, the detection wavelength is that the accelerant M is 210nm and the accelerant DPG is 205nm, the scanning wavelength range is 190-400nm, the moving phase is A-0.1% formic acid and B-0.1% formic acid- acetonitrile, the flow velocity is 0.3-0.4mL/min, the column temperature is 25-40 DEG C, the sample size is 0.1-2microliter. Through the method disclosed by the invention, the accelerant M and the accelerant DPG added in the anti-fatigue type Chinese patent medicine and healthcare food can be dedicatedly, sensitively, quickly and preliminarily screened, confirmed and quantified, and detection is mainly suitable for the accelerant M and accelerant DPG analysis in the tablet and capsule preparation.

Description

technical field [0001] The invention belongs to the field of pharmaceutical chromatography and mass spectrometry analysis, relates to a detection method of chemicals, in particular to a detection method of accelerator M and accelerator DPG in Chinese patent medicine and health food. Background technique [0002] Accelerator M (2-mercaptobenzothiazole, CAS number: 149-30-4, molecular formula: C 7 h 5 NS 2 , Molecular weight: 167.0) is an accelerator for natural rubber and synthetic rubber in the industry. It can be used alone or in combination with sulfurized carbamates, thiurams, guanidines, and other alkaline accelerators. It has a rapid acceleration effect on natural rubber and general sulfur-sulfurized synthetic rubber. The critical temperature of sulfuration is low, and it is easy to disperse in rubber and does not pollute. Mainly used in the manufacture of tires, tapes, rubber shoes and other industrial rubber products. Exposure accelerator M may cause allergic skin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 贾昌平赵琪张珊珊张斌郑佳新郑梅陈丽波钱叶飞
Owner 苏州市药品检验检测研究中心
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