LC-Q-TOF/MS detection technology for 544 pesticide residues in stone fruits
A Q-TOF, pesticide residue technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of high price, loopholes in food safety monitoring, and only 2 or 3 years of validity, and achieve the effect of large amount of information
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Embodiment 1
[0066] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in stone fruit (taking peach as an example), including the following steps:
[0067] 1. Specific steps of sample pretreatment technology:
[0068] 1.1 Take the edible part of the peach sample, chop it up, mix it evenly, seal it, and mark it;
[0069] 1.2 Weigh 10g of peach sample (accurate to 0.01g), add 40mL of 1% acetic acid acetonitrile into an 80mL centrifuge tube, use a high-speed homogenizer at 13500r / min, homogenize and extract for 1min, add 1g of sodium chloride, 4g of anhydrous magnesium sulfate , shake for 5 min, centrifuge at 4200 r / min for 5 min, take 20 mL of the supernatant, concentrate it to about 1 mL by rotary evaporation in a 40°C water bath, and wait for purification.
[0070] 1.3 in Carbon / NH 2 Add about 2cm high anhydrous sodium sulfate to the column. Rinse the SPE column with 4 mL of acetonitrile + toluene (3+1, v / v) first, and discard th...
Embodiment 2
[0099] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in stone fruit (taking apricot as an example).
[0100] The sample pretreatment steps and LC-Q-TOF / MS operating conditions refer to the processing conditions in Example 1.
[0101] Measure the sample solution in full-scan mode, compare the detection results with the TOF database, and obtain the first-level TOF score, see Figure 4 ; For compounds whose scores meet the requirements, establish a secondary acquisition method in the software, see Figure 5 ;In MS / MS mode, re-run the sample solution to obtain the full scan data of the sample fragment ions, compare it with the fragment ion information in the MS / MS library, and obtain the secondary QTOF score, see Figure 6 .
[0102] LC-Q-TOF / MS detection results in apricot samples in a certain area: 7 commercial pear samples were collected in a certain area, and 544 kinds of pesticide residues were detected by LC-Q-...
Embodiment 3
[0106] Implementation examples of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in stone fruit (jujube as an example) samples.
[0107] The sample pretreatment steps and LC-Q-TOF / MS operating conditions refer to the processing conditions in Example 1.
[0108] Measure the sample solution in full-scan mode, compare the detection results with the TOF database, and obtain the first-level TOF score, see Figure 7 ; For compounds whose scores meet the requirements, establish a secondary acquisition method in the software, see Figure 8 ;In MS / MS mode, re-run the sample solution to obtain the full scan data of the sample fragment ions, compare it with the fragment ion information in the MS / MS library, and obtain the secondary QTOF score, see Figure 9 .
[0109] LC-Q-TOF / MS detection results in jujube samples in a certain area: 9 commercially available jujube samples in a certain area were collected, and 544 kinds of pesticide residues were det...
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