Non-target quick screening and detecting method for PDE-5 inhibitor banned drugs in health foods
A PDE-5, health food technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as incomplete detection and analysis, and achieve low detection limit, small matrix effect, and good linearity
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Embodiment 1
[0025] 1. Preparation of standard solutions of 13 kinds of PDE-5 inhibitor drugs: Weigh 2.0mg of each standard PDE-5 inhibitor drug, put it in a 10mL volumetric flask, dilute to the mark with methanol, and prepare a standard stock solution of 200μg / mL . Dilute with methanol to prepare a 10 μg / mL mixed standard solution according to the needs of the experiment, dilute to prepare a series of standard working solutions, and store at 4 °C.
[0026] 2. QuEChERS technology and ultrasonic-assisted extraction pretreatment method: use the response surface experimental design method, use the Box-Behnken experimental design scheme, the four factors are, ACN:H2O ratio (, %v / v), MgSO4&NaCl dosage (, mg ), adsorbent C18 (, mg), ultrasonic time (, min), and the quadratic regression equation model predicts and evaluates the recovery rate of 13 PDE-5 inhibitors, so as to optimize the four sample pretreatment extraction factors. The table header of Box-Behnken experimental design is as follows...
Embodiment 2
[0049] Take 1mL of certain tonic wine, add 15mL of acetonitrile and water mixed solution (the volume ratio of acetonitrile and water is 7:3), mix well, add 1g of magnesium sulfate and 0.25g of sodium chloride, fully vortex on a micro mixer for 1min , sonicate for 10 minutes, centrifuge at 6000r / min for 5 minutes, transfer the supernatant to a 25mL graduated tube, and pass 1mL of the solution through a 0.45μm organic microporous nylon filter membrane for IDA-MS detection and analysis. See attached table 5 for the screening data table of PDE-5 inhibitor prohibited drugs. According to the high-resolution mass spectrometry data information, it can quickly screen and analyze the prohibited drugs in health tonic wine (attached figure 4). A sample of tonic wine contains demethylated Sildenafil is a prohibited drug ingredient.
[0050] Table 5 is the Masterviews database of 86 PDE-5 inhibitor banned drugs
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