Method for detecting unmetabolized polycyclic aromatic hydrocarbons in urine on basis of low-temperature frozen extraction technology
An extraction technology and a technology for polycyclic aromatic hydrocarbons, which are applied in the field of detecting unmetabolized polycyclic aromatic hydrocarbons in urine based on low temperature freezing extraction technology, can solve the problem of high technical cost, achieve high selectivity and sensitivity, improve the recovery rate of standard addition, The effect of improving the bonding rate
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Embodiment 1
[0029] (1) Collection of samples
[0030] Urine samples were collected from fourth-grade primary school students, and urine samples were collected from children's morning urine for three consecutive days.
[0031] (2) Experimental materials and instruments
[0032] Instruments: gas chromatography-triple quadrupole tandem mass spectrometer, nitrogen blowing instrument (ETEL4MG-2200), vortex instrument (SIVortex-2), centrifuge (DT5-2), aerosol spray generator (TSI 3079), CO2 pump.
[0033] Materials: acetonitrile, n-hexane, toluene, nonane, liquid carbon dioxide, trimethylchlorosilane, di-tert-butyl dicarbonate, sodium chloride, potassium chloride, 16 deuterated polycyclic aromatic hydrocarbon isotope standard solutions, etc., such as Unless otherwise specified, the reagents in this example are all commercially available products.
[0034] (3) Experimental method
[0035] This embodiment mainly adopts the method of detecting non-metabolized polycyclic aromatic hydrocarbons in ...
Embodiment 2
[0046] This embodiment mainly adopts the method of detecting non-metabolized polycyclic aromatic hydrocarbons in urine by low-temperature freezing extraction technology, which includes the following steps;
[0047] S1: Mix 10ml of urine specimen with 5ml of acetic acid buffer, add 1ml of 16 kinds of deuterated polycyclic aromatic hydrocarbon isotope standard solution (purchased from Wuhan Ruichen Standard Material Technology Co., Ltd.) as a recovery rate indicator, and obtain the sample to be tested; acetic acid The buffer can also be replaced by ammonium acetate buffer at a concentration of 1mol / L.
[0048] S2: adding a certain amount of pretreatment agent to the sample to be tested, using the electrode stirring head to stir at 25° C. for 3 minutes, and using the electrode to excite the pretreatment agent to pretreat the sample to be tested to obtain a pretreated urine sample; The pretreatment agent is composed of trimethylchlorosilane, di-tert-butyl dicarbonate, sodium chlor...
Embodiment 3
[0057] This embodiment mainly adopts the method of detecting non-metabolized polycyclic aromatic hydrocarbons in urine by low-temperature freezing extraction technology, which includes the following steps;
[0058] S1: Mix 10ml of urine specimen with 5ml of acetic acid buffer, add 1ml of 16 kinds of deuterated polycyclic aromatic hydrocarbon isotope standard solution (purchased from Wuhan Ruichen Standard Material Technology Co., Ltd.) as a recovery rate indicator, and obtain the sample to be tested; acetic acid The buffer can also be replaced by ammonium acetate buffer at a concentration of 1mol / L.
[0059] S2: adding a certain amount of pretreatment agent to the sample to be tested, using an electrode stirring head to stir at 22° C. for 5 minutes, and using the electrode to excite the pretreatment agent to pretreat the sample to be tested to obtain a pretreated urine sample; The pretreatment agent is composed of trimethylchlorosilane, di-tert-butyl dicarbonate, sodium chlori...
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