Pretreatment method and quantitative detection method of quinolone antibiotics in biological sample

Abstract

The invention discloses a pretreatment method and a quantitative detection method of quinolone antibiotics in a biological sample. The method is characterized by comprising the steps of putting a biological sample to be detected into a glass centrifuge tube, adding a 10 mmol / L phosphate buffer solution of which the volume is 10 times that of the sample liquid to be detected and the pH value is 6,and uniformly mixing to obtain a uniform solution; adding a TiO2-Tb nano material into a uniform solution; performing ultrasonic-assisted extraction for 3 to 8 minutes; centrifuging and discarding anupper-layer solution; adding an acetic acid solution with the mass concentration of 4wt% into a lower-layer solution, wherein the volume of the acetic acid solution is equal to that of the phosphate buffer solution; and performing ultrasonic-assisted back extraction for 12 to 18 minutes, centrifuging, taking an upper-layer solution, filtering with a 0.45 mu m microporous filter membrane, and applying the upper-layer solution to high performance liquid chromatography-ultraviolet spectrophotometric quantitative detection of quinolone antibiotics. The method has the advantages of simplicity, quickness, high target recovery rate, high sensitivity and good accuracy.

Description

technical field [0001] The invention relates to a pretreatment method of antibiotics, in particular to a pretreatment method of quinolone antibiotics in biological samples and a quantitative detection method thereof. Background technique [0002] Existing pretreatment methods for quinolone antibiotics in biological samples include liquid-liquid extraction, solid-phase extraction, and solid-phase microextraction. However, the traditional liquid-liquid extraction requires a large amount of organic reagents, and requires multiple extractions to complete the extraction, and the operation is cumbersome; and although solid-phase extraction is a classic extraction method, it requires solid-phase extraction equipment and solid-phase extraction equipment. Phase extraction cartridges, solid phase extraction cartridges are expensive, and reproducibility problems will affect the accuracy of subsequent determinations; in addition, subsequent solid phase extraction needs to be concentrate...

AI Technical Summary

Problems solved by technology

However, the traditional liquid-liquid extraction requires a large amount of organic reagents, and requires multiple extractions to complete the extraction, and the operation is cumbersome; and although solid-phase extraction is a classic extraction method, it requires solid-phase extraction equipment and solid-phase extraction equipment. Phase extraction cartridges, solid phase extraction cartridges are expensive, and reproducibility problems will affect the accuracy of subsequent determinations; in addition, subsequent solid phase extraction needs to be concentrated with a nitrogen blower, the entire extraction process takes a long time and requires A large amount of organic reagents are used for column flushing and sample elution; although solid-phase microextraction is a micro-extraction method, it requires special equipment, which is expensive, and the service life of the extraction fiber has always been longer than that of previous treatment methods. application constraints

In summary, the current determination of quinolone antibiotics in biological samples must undergo certain pretreatments before sample pretreatment, such as protein precipitation, etc. These processes are time-consuming, labor-intensive, cumbersome to operate, and consume a lot of organic solvents. Moreover, increasing the operation steps will reduce the recovery rate of the subsequent determination and affect the accuracy of the determination, which will lead to insufficient stability and reliability of the back-end detection results.

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