Method for splitting and measuring enantiomer of chiral pesticide benalaxyl through ultra-performance convergence chromatography-tandem mass-spectrometric technique
An ultra-efficient phase convergence and tandem mass spectrometry technology, which is applied in the resolution and quantification of racemates, can solve the problems of cumbersome synthesis of chiral columns, long separation time, and consumption of organic solvents, etc., to achieve separation and fast analysis speed , the effect of high sensitivity
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example 1
[0031] 1. Instruments and reagents:
[0032] Tert-butyl methyl ether, methanol and isopropanol are chromatographic grade reagents, sodium citrate and sodium chloride are analytical reagents; distilled water meets the requirements of first-grade water in GB / T 6682.
[0033] Waters TQD quadrupole tandem mass spectrometer; water bath constant temperature oscillator; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).
[0034] 2. Sample handling:
[0035] Accurately weigh 2 g of the ground grain sample into a 50 mL capped centrifuge tube, add 10 mL of water, add 10 mL of acetonitrile after soaking, then place the centrifuge tube on a vortex mixer and vibrate at 2000 rpm for 5 min. Then add 5 g of anhydrous magnesium sulfate, 1 g of sodium chloride, 1 g of sodium citrate and 0.5 g of disodium hydrogen citrate to the centrifuge tube, and immediately oscillate at a rate of 2000 rpm for 5 min, then centrifuge at 6000 rpm for 3 min; pipette 1.0 mL of the supernatant into...
example 2
[0042] As described in Example 1, another tobacco sample was selected, and the contents of S-benalaxyl and R-benalaxyl in the sample were 0.85 and 0.74 mg / kg, respectively.
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