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(1) Liquid chromatography conditions
Column: IntersilC 18 , 3μm, 150mm×2.
1mm or equivalent; injection volume: 20μL; flow rate: 0.
5mL/min; column temperature: 20℃; mobile phase: A: 0.
1mmol/L ammonium formate solution, B: Acetonitrile
.
The gradient elution conditions are shown in Table 6-3
Table 6-3 Gradient elution conditions
(2) Mass spectrometry conditions
Ion source: electrospray ion source; scanning method: positive ion scanning; detection method: multi-reaction monitoring; electrospray voltage: 5500V; atomizing gas pressure: 0.
069MPa; curtain air pressure: 0.
69MPa; auxiliary gas flow rate: 0.
414MPa; Ion source temperature: 350°C; collision cell outlet voltage: 2.
0V; qualitative ion pair, quantitative ion pair, collision energy and declustering voltage, see Table 6-4
.
Table 6-4 Qualitative ion pair, quantitative ion pair, collision energy and declustering voltage of 9 antibiotics
(3) Qualitative determination
Under the same experimental conditions, the ratio between the retention time of the analyte in the sample solution to be tested and the retention time of the analyte in the matrix standard working solution is within ±2.
5%
.
In addition, in the sample solution to be tested, the relative abundance of each qualifier ion in the test substance is close to the ratio of the relative abundance of each qualifier ion in the matrix standard working solution of the test substance with a concentration close to the ratio, and the deviation does not exceed the range specified in Table 1-5 , It can be determined that there is a corresponding analyte in the sample
(4) Quantitative determination
Under the best working conditions of the instrument, draw a standard working curve with the concentration of the matrix standard working solution as the abscissa and the peak area as the ordinate
.
Use the working curve of the matrix standard working solution to quantify the sample.
