Method for detecting nitromidazole residue in royal jelly by using high performance liquid chromatography tandem mass spectrum

Abstract

The invention relates to a method for detecting the nitromidazole residue in royal jelly by using a high performance liquid chromatography tandem mass spectrum. At present, a detection method with less consumption of reagents, low detection cost and high detection sensitivity is not found. The method comprises the work procedures of standard solution preparation, royal jelly sample treatment, standard curve preparation and royal jelly sample detection, wherein the work procedure of royal jelly sample treatment comprises the following steps of: removing protein and other polar compounds in a royal jelly sample with 2 percent HCCLO4; adjusting the pH value of supernate to be 8.8 with 1mol / L NaOH so as to enable organic acid and alcohol soluble protein in the supernate to salinize, improve the polarity, and prevent being extracted by ethyl acetate; and finally obtaining the residual quantity of nitromidazole medicaments from the detection sample solution by using a high performance liquid chromatography and a trebling quadrupole rod tandem mass spectrum. The invention has less consumption of reagents and low detection cost and the detection limits of metronidazole, ronidazol and dimetrdazole are respectively 0.03mu g / kg, 0.06mu g / kg and 0.03mu g / kg.

Description

technical field [0001] The invention relates to a method for measuring nitroimidazole residues in royal jelly, in particular to a method for measuring nitroimidazole residues in royal jelly by high performance liquid chromatography tandem mass spectrometry. It is mainly used to determine the residual amount of metronidazole, ronidazole and dimetidazole in royal jelly. Background technique [0002] The chemical structure of nitroimidazoles is characterized by an imidazole ring with a nitro group at the fifth position in the molecule. Nitroimidazoles have broad-spectrum antibacterial and antiprotozoal effects, and are common clinical drugs. [0003] The liquid chromatography-tandem mass spectrometry method has been widely used by government supervision and inspection agencies at home and abroad as a confirmation method. The liquid chromatography-tandem mass spectrometry method has unique advantages in sensitivity, accuracy, and detection efficiency, and has become the most sup...

AI Technical Summary

Problems solved by technology

However, due to the complex matrix of royal jelly and the difficulty in sample purification, the accuracy of the liquid chromatography-tandem mass spectrometry method for the determination of nitroimidazoles in royal jelly is not high. The detection standard of the most advanced level of imidazole drug detection technology. In GB / T 23407-2009, the determination of nitroimidazole drug and its metabolite residues in royal jelly uses liquid chromatography-mass spectrometry / mass spectrometry, but GB / T The detection limit of T 23407-2009 assay method is 2.0μg / kg

[0004] At present, the EU requires that drug residues in animal-derived foods should not be detected, that is, below the detection limit of the detection method. The detection limit of nitroimidazoles in royal jelly freeze-dried powder in the EU has reached 2.5 μg / kg. The detection limit of nitroimidazoles has reached 0.5 μg / kg. Since then, the standard method in my country’s GB / T 23407-2009 can no longer meet the requirements, and the methods reported in other similar literatures are far from the above. The requirements of the detection limit, such as the high-performance liquid chromatography-tandem mass spectrometry published in the chromatographic volume 24, the 4th, 331-334 pages in 2006 by Ding Tao, Xu Jinzhong, Shen Chongyu, etc. Determination of three kinds of nitroimidazoles in royal jelly Residues can not meet the requirements of the above detection limit

Moreover, due to the complex composition of the sample matrix of bee products, in order to reduce the matrix effect, solid phase extraction technology has been adopted in many liquid chromatography-mass spectrometry / mass spectrometry methods, such as nitroimidazoles and nitroimidazoles in royal jelly in GB / T 23407-2009 Determination method of its metabolite residues, SN / T 1928-2007 Detection method of nitroimidazole residues in food of animal origin for import and export, Announcement No. 1025 of the Ministry of Agriculture-22-2008 Detection of 4 kinds of nitroimidazole residues in food of animal origin Method and HPLC-APCI(+) MS / MS analysis of nitroimidazoles in food of animal origin published by Yin Juyi, Xie Donghua, Li Zuoqing, etc. Solid-phase extraction technology is used in the methods of drug residues, which increases the detection cost

[0005] In summary, there is currently no method for measuring nitroimidazole residues in royal jelly by high performance liquid chromatography tandem mass spectrometry that is simple, has low reagent consumption, low detection cost, high detection efficiency, good accuracy, and high sensitivity

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