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5.
2.
4.
6 Determination
(1) Liquid chromatography conditions
Chromatographic column: SunFire TM C 18 3.
5 um, 150 mm×2.
1 mm (inner diameter) or equivalent; see Table 5-26 for mobile phase and flow rate; column temperature: 30°C; injection volume: 20 μL
.
Table 5-26 Liquid chromatography gradient elution conditions
(2) Mass spectrometry conditions
Ion source: Electrospray ion source (ESI); Scan mode: Positive ion scan; Detection mode: Multi-reaction monitoring: Electrospray voltage: 5500V; Atomizing gas pressure: 0.
055 MPa; Curtain gas pressure: 0.
079 MPa; Auxiliary gas flow rate: 6 L/min; ion source temperature: 400℃; qualitative ion pair, quantitative ion pair and declustering voltage (DP), focus voltage (FP), collision energy (CE) and collision cell exit voltage (CXP) are shown in Table 5- 27
.
Table 5-27 Qualitative ion pair, quantitative ion pair, declustering voltage, focusing voltage, collision gas energy and collision cell exit voltage of 6 penicillins
(3) Qualitative determination
Under the same experimental conditions, if the test substance in the sample has the same retention time as the standard substance tested at the same time, and the selected two pairs of ion abundance ratios are consistent, it can be determined that the residue is present in the sample
.
(4) Quantitative determination
Under the best working conditions of the instrument, the matrix mixed standard solutions prepared by penicillin G, penicillin V, naphthalene penicillin , oxacillin , o-chloropenicillin , and dicloxacillin standard stock solutions were used to inject samples respectively with the standard working solution concentration It is the abscissa and the peak area is the ordinate to draw a standard working curve
.
Use the standard working curve to quantify the sample.
The response values of penicillin G, penicillin V, ethoxynene penicillin, oxacillin, o-cloxacillin, and dicloxacillin in the sample solution should all be within the linear range determined by the instrument
Under the above chromatographic conditions, the total ion current diagrams of penicillin G, penicillin V, naphthalene penicillin, oxacillin, o-cloxacillin, and dicloxacillin are shown in Figure 5-7, and the retention time and ion abundance ratio are shown in Table 5- 28
Table 5-28 Retention time and ion abundance ratio of 6 penicillins
Figure 5-7 Total ion current diagram of 6 penicillin standard substances
Related Links: Determination of 6 Penicillin Residues in Honey Application Scope and Method Principles of Liquid Chromatography-Tandem Mass Spectrometry