MS-CLEAN VDR
The pretreatment products of MS clean VDR, combined with hydrophobic action and acid-base theory, can selectively capture phospholipid interferences that lead to ion inhibition without affecting the loss of target substances, provide excellent purification effect for fat containing samples, improve the sensitivity of the instrument to detect analytes, and reduce the maintenance cost of the instrument to a large extentProduct features
● effectively remove phospholipid and reduce ion inhibition effect
● one time treatment of multiple animal residues, saving time
●No need for activation, rinsing, easy operation and stable recovery
●More pure sample, cleaner mass spectrum source, less data error
Prat No |
Specifications |
packing |
MSV330 |
MS- -clean VDR, 300 mg/3 mL |
50branch |
202002-2110 |
Target-core C18 (2.1mmx100 mm, 2.7 um) |
1root |
MSi2500 |
MS-Mix Multifunctional mixer |
1platform |
Analysis of 19 veterinary drug residues in pork by UPLC / MS / MS
1 sample extraction
1) Weigh 2.0g pork into a 50ml centrifuge tube, add 2.0ml of 0.1M nazedta mcllvaine buffer solution, mix with vortex for 1min, extract with ultrasonic wave in ice bath for 10min, centrifuge for 5min at 4 ° C 9000r / min, and transfer it to another 15ml centrifuge tube; 2) add 7.0ml of 2% ethyl formate into a 50ml centrifuge tube, vortex for 5min, and centrifuge for 5min at 4 ° C 9000r / min, Combine the supernatant twice, and use 2% ethyl formate to fix the volume to 10m L; 3) centrifugate the supernatant after the volume is fixed at 4 ° C 9000r / min for 5min, to be purified!
2 sample purification
1) Sample loading: take 2.5ml of the solution to be purified to pass through the column, and then put it into prison under the action of gravity, so as to make the effluent deaf; 2) elute: add 625 "80% acetonitrile water for secondary elution, collect the effluent, apply Zhendeng e empty liquid, and combine the effluent twice; 3) add 0.5ml of the sample eluent and 0.3ml of HQ into the sample bottle, vortex and mix well, and pass through 0.22 μ m organic filter membrane for on-board test.
3 preparation of standard Koji
The standard koji was prepared with empty matrix and quantified by internal standard method. The concentration range of standard koji was 0.5-100ppb
4. Instrument test conditions
(for reference only) chromatographic condition instrument: UPLC / MS / MS (Thermo Fisher TQS Endura) chromatographic column: target core C18 (2.1mmx50 mm, 1.8 PM) column temperature: 30 ° C
Injection volume: 8 pl
Flow rate: 0.4ml/min
Mobile phase: A: water (0.1% formic acid) B: methanol (0.1% formic acid)
Table 1 gradient elution
Mass spectrometry conditions
Ion source: HESI sheath gas pressure: 40 ARB ion transfer tube: 380 ° C
Electrospray voltage: 3500 V auxiliary gas pressure: 2 ARB auxiliary gas temperature: 420 degrees C
matter
1. In order to prevent the loss of tetracycline compounds caused by chelation, aqueous extraction was carried out with 0.1M Na2EDTA buffer solution.
2. In order to improve the phase separation from solid residues, it is recommended to use low temperature centrifugation (4 ° C) to reduce the impact of temperature on some targets (such as tetracyclines).
3. High speed centrifugation (9000r / min) is recommended to further ensure the effective removal of protein and some solid residues
4. It is suggested to add internal standard and prepare standard curve with blank matrix, which is helpful to correct the recovery of target analyte
experimental result
Table 2. Experimental results of recovery of 19 kinds of animal residues in pork of different brands with standard addition concentration of 16ng / ml, n = 3