Method for measuring residual quantity of chloramphenicol in serum through liquid chromatography-tandem mass spectrometry
A method of determination, liquid chromatography technology, applied in the field of liquid chromatography-tandem mass spectrometry determination of chloramphenicol residues in serum, can solve the problems of small sampling volume, cumbersome operation, easy introduction of pollution, etc., and achieve fast chromatographic separation , Quantitative, reliable, and specific effects
Inactive Publication Date: 2009-09-09
王磊
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[0005] The detection of residual chloramphenicol in serum can adopt analytical methods such as microbiological method, immune method, radioimmunoassay, GC, HPLC, GC-MS, etc., but the sensitivity of the detection method is mostly difficult to meet the requirements of small sampling volume, accuracy and high sensitivity. In recent years, with the rapid development of chromatographic technology, it is possible to carry out highly sensitive quantitative analysis of chloramphenicol residues in serum
[0006] In the current chromatographic-tandem mass spectrometry detection of chloramphenicol residues, either the external standard method is used for quantification, or the unextracted chloramphenicol standard sample is used as the quantitative standard, which affects the reliability of the detection results
Simultaneously, because of its sample pretreatment adopts the method that multiple liquid-liquid extraction, solid-phase extraction or liquid-liquid extraction and solid-phase extraction combine, its operation is loaded down with trivial details expense, and easily introduces pollution, and the chromatographic separation of chloramphenicol and It takes a certain amount of time, so it is difficult to meet the needs of actual work, especially a large number of batch detection and analysis
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[0028] 1. Sample processing method (liquid-liquid extraction): Accurately extract 0.6ml blank serum sample with a pipette, accurately add 0.4ml methanol solution and 50μL internal standard working solution (deuterated chloramphenicol, D5), shake and mix, Centrifuge at 6000r / min for 5 minutes, take the supernatant and filter it through a 0.45μm filter membrane before testing.
[0029] 2. Liquid chromatography conditions (gradient elution):
[0030] a) Chromatographic column: THEMO HYPERSIL GOLD C18, 5 μm, 150×2.1 mm.
[0031] b) Mobile phase ratio and gradient setting: choose ammonium acetate solution as the aqueous phase; methanol as the organic phase; see Table 1 for gradient elution.
[0032] Table 1 Mobile phase gradient elution program
[0033]
[0034]
[0035] c) The column temperature is 25°C.
[0036] d) The injection volume is 20 μL.
[0037] 3. Mass Spectrometry Conditions
[0038] ①Ionization mode: Atmospheric pressure electrospray ion source (ESI), posit...
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Abstract
The invention relates to a method for measuring the residual quantity of chloramphenicol through liquid chromatography-tandem mass spectrometry, in particular to a method for measuring residual trace chloramphenicol in human serum and animal serum through the liquid chromatography-tandem mass spectrometry. The aim of the invention is to establish a feasible and universal method for rapidly and effectively carrying out quantitative measuration on the chloramphenicol in the serum, which can well meet the requirement of practical work. The established liquid chromatography-tandem mass spectrometry method uses deuterated chloramphenicol as an interior label, uses an interior label method to quantify residual chloramphenicol in the serum and can correct various errors possibly produced in the full process of sample analysis comprising sample pretreatment, chromatographic resolution and mass spectrometric detection. The method has the advantages that: in the sample pretreatment, a simple liquid-liquid extraction method is adopted to purify and enrich the chloramphenicol in the serum; and in the chromatographic resolution of samples, a short chromatogram column with small caliber and an isocratic or gradient elution method are adopted to realize rapid chromatographic resolution of the chloramphenicol.
Description
technical field [0001] The invention relates to a method for measuring residual chloramphenicol in organisms, more specifically a method for quantitatively determining trace amounts of residual chloramphenicol in human and animal serum. Background technique [0002] Chloramphenicol is a relatively cheap and effective broad-spectrum antibiotic, which mainly inhibits the combination of bacterial 70S ribosomes and 50S subunits and interferes with bacterial protein synthesis to produce antibacterial effects. In its use for more than 50 years, it has been effectively used in the treatment of various infectious diseases in humans and animals, but years of clinical application have shown that chloramphenicol has relatively large toxic and side effects on humans, and its role is due to the carbonyl group in its structure. It is caused by a connected CHCl2 group, which can cause the human body to produce irreversible bone marrow hematopoietic dysfunction diseases-aplastic anemia and ...
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Login to View More IPC IPC(8): G01N30/02G01N30/34G01N30/60G01N30/08G01N30/50G01N30/72
Inventor 王磊
Owner 王磊