Array chip mass spectrometry analysis method of photoelectrochemical reaction intermediate

[0027] Example 1

[0028] A titanium dioxide-modified array chip is used in conjunction with electrostatic spray ionization mass spectrometry to detect the intermediates in the photooxidation reaction of mitoxantrone. It includes the following steps:

[0029] Take 0.1g of Degussa P25 titanium dioxide, grind it in a mortar for 1 hour, add 1 ml of 1% acetic acid dropwise during the grinding process, disperse the ground titanium dioxide powder in 1 ml of ethanol, and dilute it 25 times in water to obtain 4 Milligrams per milliliter of titanium dioxide suspension. The suspension is modified on the glass surface using inkjet printing technology to form an array chip. The chip was burned at 400 degrees Celsius for one hour and then naturally cooled.

[0030] 0.4 millimoles per liter, 1 microliter of mitoxantrone aqueous solution was dropped on the surface of the glass plate modified with titanium dioxide, and it was directly detected by electrostatic spray ionization mass spectrometry. The square wave pulse high voltage used in the detection was 0- 6 kV, 100 Hz. Get as figure 2 In the spectrum shown, the peak with a mass-to-charge ratio of 445 is the peak of protonation of mitoxantrone.

[0031] The glass slide with mitoxantrone and modified with titanium dioxide was irradiated under an ultraviolet lamp, and different time points were used for electrostatic spray ionization mass spectrometry detection. The square wave pulse high voltage used in the detection was 0-6 kV. 100 Hz. Get as image 3 In the spectrum shown, the peaks with mass-to-charge ratios of 442, 443, 459, 475, 489 are the protonation peaks of the intermediates of the photocatalytic oxidation product of mitoxantrone. Among them, A is the mass spectrum of mitoxantrone in the electrostatic spray ionization mass spectrum after being irradiated with a UV lamp for 1 minute, B is the mass spectrum of mitoxantrone in the electrostatic spray ionization mass spectrum after being irradiated by a UV lamp for 3 minutes, and C is The mass spectrum of mitoxantrone in electrostatic spray ionization mass spectrometry after 5 minutes of ultraviolet lamp irradiation, and the mass spectrum of mitoxantrone in electrostatic spray ionization mass spectrometry after ultraviolet lamp irradiation for 10 minutes.

[0032] Example 2

[0033] A graphene-modified polyimide array chip was used in conjunction with electrostatic spray ionization mass spectrometry to detect the intermediates of the photooxidation reaction of mitoxantrone.

[0034] Graphene oxide ink formula: Add 3 mg of graphene oxide flakes (Nanjing Xianfeng Nano Material Technology Co., Ltd.) and 50 mg of polyvinylpyrrolidone (PVP) powder to 1 ml of water: isopropanol (3:1) mixture, and Ultrasound in an on/off cycle with an amplitude of 35% in a 2 ml centrifuge tube for 180 minutes. The final dispersion concentration is 3 mg/ml graphene oxide. Then, put the dispersion in a centrifuge at 13000 g Centrifuge for 20 minutes and remove the supernatant. Thereafter, the precipitate was redispersed in 1 ml of 1,2-propanediol-based mixture, which contained 10% terpineol.

[0035] An inkjet printer was used to print the above ink on the surface of a polyimide substrate (0.2 mm thickness) to form an array of dots with a diameter of 0.2 mm, and the printing layer was stabilized by light curing.

[0036] Drop 0.4 millimoles per liter, 1 microliter of mitoxantrone aqueous solution on the polyimide array chip modified with graphene oxide, and directly detect it by electrostatic spray ionization mass spectrometry. The square wave used in the detection The pulse high voltage is 0-6 kV, 100 Hz. A peak with a mass-to-charge ratio of 445 was detected, which is a peak of protonation of mitoxantrone.

[0037] The polyimide array chip with mitoxantrone and modified with graphene oxide was irradiated under an ultraviolet lamp, and the electrostatic spray ionization mass spectrometry was performed at different time points within 0-30 minutes. The square wave pulse high voltage is 0-6 kV, 100 Hz. The peaks at 442 and 443 are the protonation peaks of the intermediates of the photocatalytic oxidation product of mitoxantrone.