Method for simultaneously measuring residual quantities of lincomycin and macrolides in royal jelly

Abstract

The invention relates to a method for simultaneously measuring residual quantities of lincomycin and macrolides in royal jelly by a liquid chromatography and a tandem mass spectrometer. Currently, the prior method can not achieve the goals of low detection cost and a detection limit less than 1 mu g / kg. The method comprises the steps of standard solution preparation, royal jelly sample treatment,standard curve making and royal jelly sample detection; in the step of royal jelly sample treatment, acetonitrile ammonia water with the volume concentration of 97% is used as the extracting solution, residues in a 50 ml glass centrifuge bottle after vacuum concentration are transferred by a phosphate buffer solution and mixed with ethyl acetate so as to carry out extraction; and finally, the detection sample solution is measured by a high performance liquid chromatograph and a ternary quadrupole tandem mass spectrometer to obtain the residual quantities of lincomycin and macrolides in royal jelly. The invention has the advantages of low detection cost and high detection efficiency, the detection limit reaches 0.2-0.9 mu g / kg, and the linearly related coefficient is 0.9914-0.9994.

Description

technical field [0001] The invention relates to a method for simultaneous determination of lincomycin and macrolide residues in royal jelly, in particular to a method for simultaneous determination of lincomycin and macrolides in royal jelly by using liquid chromatography tandem mass spectrometry residual method. Background technique [0002] Lincomycin (LIN) is a class of alkaline antibiotics produced by Streptomyces lincolnensis. It is effective against most Gram-positive bacteria and some anaerobic Gram-negative bacteria, and can cause elevated transaminase and Jaundice, can cause allergic reactions, can cause hypotension or cardiac arrest, can cause tinnitus, dizziness and other reactions. Macrolides (Macrolides, MALs) are a class of antibacterial drugs with a common chemical structure of a 14- or 16-membered carbon lactone ring, mainly acting on aerobic Gram-positive and negative cocci, anaerobic bacteria, and Legionnaires. Bacteria, Campylobacter fetus, Chlamydia and...

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Problems solved by technology

[0004] It can be seen from the above that the liquid chromatography-tandem mass spectrometry method has been widely used by domestic and foreign government supervision and inspection agencies as a confirmation method. For all samples, the detection limit can meet the requirements. For example, the matrix of royal jelly is complex and the sample purification is difficult. The detection method of macrolide antibiotic residues in royal jelly imported and exported in SN / T 2062-2008 is the macrolide antibiotic residue in royal jelly. According to the inspection standard for the import and export of cyclic lactone drugs, the detection limit is 10 μg / kg. However, if the current enterprise wants to export royal jelly freeze-dried powder, the residual amount of macrolide antibiotics in the raw material royal jelly must be controlled at 3 μg / kg Only in this way can the export requirements of royal jelly freeze-dried powder be met, which leads to the detection method of macrolide antibiotic residues in royal jelly imported and exported in SN / T 2062-2008 is far from meeting the requirements. Other literature reports Some detection methods have adopted solid-phase extraction technology, such as the high-performance liquid chromatography tandem mass spectrometry method in the determination of animal tissue by Yue Zhenfeng, Chen Xiaoxia, Xie Liqi, etc. Lincosamides and macrolide antibiotics remain, which increases the detection cost; and some simply use acetonitrile and other solvents for simple extraction, resulting in more impurities in the sample solution and a large matrix effect, which cannot reach the target of royal jelly. Required detection limit for macrolide antibiotic residues, therefore not suitable for detection of macrolide antibiotic residues in royal jelly

[0005] In summary, there is currently no method for the simultaneous determination of lincomycin and macrolide residues in royal jelly that is simple, low in detection cost, high in detection efficiency, and has a detection limit of less than 1 μg / kg. It is difficult to meet foreign requirements for lincomycin and macrolide residue limits in the detection of royal jelly

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