LC-Q-TOF/MS detection technique for 544 pesticide residues in citrus fruits
A Q-TOF and pesticide residue technology, applied in the field of food hygiene and agricultural product safety inspection, can solve the problems of high price, loopholes in food safety monitoring, valid period of only 2 or 3 years, etc., and achieve 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 citrus fruits (taking orange as an example), including the following steps:
[0067] 1. Specific steps of sample pretreatment technology:
[0068] 1.1 Take the edible part of the orange sample, chop it up, mix it, seal it, and mark it;
[0069] 1.2 Weigh 10g of orange 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 2em high anhydrous sodium sulfate to the column. Rinse the SPE column with 4 mL of acetonitrile + toluene (3+1, v / v) first, and discard t...
Embodiment 2
[0100] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in citrus fruits (Take Tangerine as an example).
[0101] The sample pretreatment steps and LC-Q-TOF / MS operating conditions refer to the processing conditions in Example 1.
[0102] 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 .
[0103] LC-Q-TOF / MS detection results in tangerine samples in a provincial capital city: 5 commercially available tangerine samples in a provincial capital city were collected, and 544 kinds o...
Embodiment 3
[0107] Implementation example of LC-Q-TOF / MS detection and confirmation technology for 544 pesticides (see Table 1) in citrus fruits (lemon as an example).
[0108] The sample pretreatment steps and LC-Q-TOF / MS operating conditions refer to the processing conditions in Example 1.
[0109] 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 .
[0110] LC-Q-TOF / MS detection results of lemon samples in a provincial capital city: 9 commercially available lemon samples in a provincial capital city were collected, and 544 kinds of pesticide resid...
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