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8.
1.
4.
2 Determination method
There are many reports on the detection methods of ASs residues in animal-derived matrices, mainly immunoassay and chromatography
.
Immunoassay methods mainly include enzyme-linked immunoassay (ELISA), radioimmunoassay (RIA) and colloidal gold immunoassay (GICA); chromatographic analysis methods mainly include gas chromatography (GC), gas chromatography mass spectrometry (GC-MS) ), High Performance Liquid Chromatography (HPLC) and Liquid Mass Spectrometry (LC-MS)
(1) Gas chromatography (gaschromatography, GC)
GC uses gas as the mobile phase for the detection of residual drugs.
It has the characteristics of high efficiency, high selectivity, high sensitivity, fast analysis speed and wide application range
.
For ASs residue analysis, there have been related reports earlier, but it has been gradually replaced by GC-MS methods
(2) Gaschromatography-mass spectrometry (GC-MS) GC-MS method is currently the most commonly used method in the detection of ASs residues
.
Among the standard methods promulgated by various countries, GC-MS is usually used as the final confirmation method
1) Electron ionization (EI)
Fritsche et al.
established a GC-MS method for the detection of androgens and estrogen in cattle muscle tissue
.
After the polar ASs are extracted by the methanol-water mixture, they are purified with a C 18 SPE column, while the non-polar ASs need to be further purified with an amino column, and finally mixed with MSTFA-TMIS-DTE (1000+2+2, v/v ) Silylation derivatization, GC-MS determination
Kootstra et al.
established a GC-MS method for multi-residue detection of ASs in urine
.
Two different derivatization reagents are used: HFBA and TMS, which are mainly used for qualitative and semi-quantitative analysis of low-dose ASs
Figure 8-4 19-norandrosterone carbonyl derivatization reaction and its products
Figure 8-5 The derivatization reaction of 19-norandrosterone hydroxyl group and its products
Yamada et al.
reported the simultaneous detection of major metabolites of anabolic steroids in horse urine using GC-MS/MS
.
After urine is β- gluconic acid hydrolysis the aldehyde, using Sep-Pak C18 PlusSPE, purified, and then the azido trimethylsilyl derivatization after, GC-MS / MS ion source EI source, detected in MRM mode
Impens et al.
established a gas chromatography-ion trap mass spectrometry (GC-MSn) detection method for ASs in bovine urine
.
Separate with a non-polar BPX-5 column (25m×0.
2) Chemical ionization (CI)
China's national standard GB/T22967-2008 uses GC-negative chemical ionization (NCI)-MS to detect β-estradiol residues in milk and milk powder
.
After the sample is hydrolyzed by β-glucuronidase and arylsulfatase and purified by HLBSPE column, it is derivatized with pentafluorobenzoyl chloride (stored at 60°C for 15 minutes), and then measured by GC-NCI-MS in SIM mode.
Some GC-MS residue detection methods for ASs in animal-derived matrices are shown in Table 8-5
.
Table 8-5 Some GC-MS residual detection methods for ASs in animal-derived matrices
Related Links: Analytical Technology of Steroid Anabolic Hormone Drug Residues-Pretreatment Methods (4)