Method of quickly analyzing illegal addition of sildenafil analogue in yang-reinforcing health care products
A rapid analysis technology for sildenafil, which is applied in the fields of material analysis, material excitation analysis, material analysis by optical means, etc.
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Embodiment 1
[0084] In this embodiment, the software used includes: drug design platform Discovery Studio 3.0; GAUSSIAN09 program package.
[0085] In this embodiment, the equipment used includes: a portable Raman spectrometer (BWS415, B&W Tek Inc., the United States), with an excitation wavelength of 785nm and a resolution of 5cm -1 , spectral coverage 175-3200cm -1 ; WFH-203B three-purpose UV analyzer (Shanghai Jingke Industrial Co., Ltd.); ultrasonic instrument (KUDOS-SK5200HP, China); centrifuge (HERAEUS, FRESCO 17Centrifuge; Thermo Scientific, USA); analytical balance (METTLER AE240, China) ; Standard spectrum processing software OPUS 5.0.
[0086] In this embodiment, the materials used include: thin-layer chromatography separation plate F 254 (10×20cm) (Merck, Darmstadt, Germany); silver nitrate and trisodium citrate (AR, Sinopharm Chemical Reagent Co., Ltd.); other reagents used were analytically pure, purchased from Sinopharm Chemical Reagent Co., Ltd.; chromatographically pure ...
Embodiment 2
[0157] Step A, pretreatment of the sample to be tested: Weigh 1 mg of the Chinese medicine to be tested, dissolve it in 10 ml of methanol, settle to volume for 3 minutes, vortex for 5 minutes, place it in an ultrasonic instrument, extract for 30 minutes, and centrifuge for 10 minutes (5000rpm, 4 ℃), stored in 4 ℃ refrigerator, pending inspection;
[0158] Step B, pipette 1 μL, spot on thin-layer chromatography separation plate F 254 (10×20cm) (Merck, Darmstadt, Germany), the standard sildenafil citrate, hydroxyhomoxidenafil citrate, vardenafil, pseudovardenafil, homeocid Nafil, reddenafil, and tadalafil each take 1 μl, adopt the optimized TLC development conditions, spot the sample at a distance of 1 to 2 cm from the bottom of the thin-layer plate, and use dichloromethane:acetone:ammonia=20:1.5: 0.2 (v / v) unfolded for 25min. Take it out at a distance of 7cm from the top of the thin-layer board, and let it dry, and inspect the thin-layer spots under a 254nm ultraviolet lamp. ...
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