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(4) Liquid chromatography-mass spectrometry (LC-MS)
Due to the toxicity of this class of drugs, many countries strictly control or prohibit clinical application, and have higher requirements for detection sensitivity.
However, LC-MS has high detection sensitivity and good specificity, and application reports are gradually increasing
.
The LC-MS detection of quinoline drugs and their metabolites mainly uses electrospray ionization (ESI), and two monitoring modes of positive ion and negative ion can be selected; there are also reports on the determination method using atmospheric pressure chemical ionization (APCI)
1) APCI ionization
Merou et al.
used LC-MS/MS to determine CBX, QCA and MQCA in pig, bovine muscle and pig liver
.
Chromatographic column is ODS column (150mm×4.
2) ESI ionization
A.
Negative ion detection
The metabolites of this class of drugs are acidic substances, and the negative ion mode can be selected for LC-MS detection
.
China's national standard GB/T22984-2008) detects QCA and MQCA in milk and milk powder
B.
Positive ion detection
Compared with negative ion detection, there are more reports of detection in positive ion mode
.
When detecting positive ions, acid can be added to the mobile phase to improve detection sensitivity
Hutchinson et al.
used LC-MS/MS to detect QCA in pig liver, the column was C18 (150mm×4.
60mm, 5μm), the mobile phase was methanol-water-acetic acid (40+59.
6+0.
4, v/v), and the flow rate was 1.
0mL /min, split 0.
2mL/min, mass spectrometry ESI positive ion, MRM detection
.
The ion source temperature is 150°C, the drying gas and atomizing gas are both nitrogen, and the flow rates are 500 L/h and 80 L/h, respectively
Zhang et al.
established an ultra-high performance liquid chromatography (UPLC)-ESI+-MS/MS residue analysis method for OLQ metabolite MQCA in fish tissues
.
Chromatographic column is UPLC BEH C18 (2.
Hutchinson et al.
established an LC-ESI-MS/MS confirmation method for QCA and MQCA in pig liver
.
The chromatographic column is a C 18 column (150mm×2.
C.
Positive and negative ion switching detection
It can also be switched by mass spectrometry ionization mode and detect positive and negative ions at the same time
.
Horie et al.
Related Links: Determination of Quinoxaline Drug Residues-High Performance Liquid Phase Fish Spectrometry