LC-Q-TOF/MS detection technique for 544 pesticide residues in solanaceous fruit vegetables
A Q-TOF, pesticide residue technology, applied in the fields of food hygiene and agricultural product safety testing, can solve the problems of high price, loopholes in food safety monitoring, and the validity period is only 2 or 3 years, and achieves the effect of large amount of information
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Embodiment 1
[0066] An implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in solanaceous vegetables (taking sweet pepper as an example), including the following steps:
[0067] 1. Specific steps of sample pretreatment technology:
[0068] 1.1 Take the edible part of the sweet pepper sample, chop it up, mix it evenly, seal it, and mark it;
[0069] 1.2 Weigh 10g of sweet pepper samples (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 sulfuric acid Magnesium, shake for 5min, centrifuge at 4200r / min for 5min, take 20mL of the supernatant, concentrate it to about 1mL by rotary evaporation in a water bath at 40°C, 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 + t...
Embodiment 2
[0099] Implementation examples of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in solanaceous vegetables (taking tomato 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 Image 6 .
[0102] LC-Q-TOF / MS detection results in tomato samples in a provincial capital city: 12 tomato samples sold in a provincial capital city were collected, and 544 kinds of pesticide res...
Embodiment 3
[0106] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in solanaceous vegetables (eggplant as an example).
[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 eggplant samples in a provincial capital city: 18 commercially available eggplant samples in a provincial capital city were collected, and 544 kinds...
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