Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS
A solid-phase supported, toxic substance technology, applied in the fields of analytical chemistry and material science, can solve the problem of inability to quickly screen toxic substances, and achieve the effect of eliminating adverse effects, rapid screening, and high detection efficiency
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Embodiment 1
[0035] 1. Prepare standard samples
[0036] Accurately weigh trichlorfon, parathion, diazinon, methamidophos, phorate, methyl parathion, monocrotophos, dimethoate, malathion, triazophos, Phosphate, isocarbophos, acephate, chlorpyrifos, monosultap, carbofuran, carbafur, methomyl, medicarb, aldicarb, isoprocarb, secbucarb, tetramethrin , cyfluthrin, lambda-cyhalothrin, bifenthrin, fenpropathrin, cypermethrin, fenvalerate, deltamethrin, endosulfan, triadimefon, butachlor, acetochlor, Isobacteria Urea, pentachloronitrobenzene, dicofol, fluroxypyr, fomesafen, tegrafyl, quizalofop, 4-chlorophenoxyacetic acid, hexythiazox, trichlorophenol, endosulfan, chlorothalon Each 25mg of clear, dichlorpyr, fenoxaprop-ethyl, atrazine, alachlor, and buprofezin standard substances was placed in a 10mL volumetric flask, and diluted with methanol to make a 2.5mg / mL standard stock solution .
[0037] Preparation of standard working solution: Accurately measure 100 μL and 50 μL of standard stock so...
Embodiment 2
[0051] Add the standard substances of various toxic substances in Table 1 to methanol respectively, wherein the added concentration of each standard substance is controlled to be 1 μg / mL, and then carry out gas chromatography-mass spectrometry analysis according to the analysis method of Example 1 to obtain the detection of each toxic substance Sensitivity, the results are shown in Table 1. The results in Table 1 show that the gas chromatography-mass spectrometry method of the present invention can simultaneously detect more than 130 toxic substances with different structures, and the detection sensitivity is 0.1-10 ng / μL.
[0052] Table 1 The detection sensitivity of each toxic substance in gas chromatography-mass spectrometry
[0053]
[0054]
[0055]
[0056]
[0057] Note: "-" means not detected.
Embodiment 3
[0059] Add the standard substances of various toxic substances in Table 3 to methanol respectively, and control the addition concentration of each standard substance to be 1 μg / mL, and then use liquid chromatography-mass spectrometry to perform liquid chromatography-mass spectrometry analysis. The analysis conditions are as follows:
[0060] Chromatographic conditions:
[0061] Chromatographic column: ACQUITYUPLC HSS C18 column, 2.1mm×150mm, 1.8μm;
[0062] Mobile phase: A: 0.1% formic acid acetonitrile, B: 5 mM ammonium formate (adjust pH to 3.5 with 0.1% formic acid)
[0063] Elution: Gradient elution, the conditions are shown in Table 2;
[0064] Column temperature: 35°C;
[0065] Flow rate: 0.4mL / min;
[0066] Table 2 Gradient elution conditions used in liquid chromatography-mass spectrometry analysis
[0067] time (min)
A(%)
B(%)
0
13
87
0.5
13
87
10
50
50
10.75
95
5
12.25
95
5...
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