Finger-print detection method for amino acid ingredients in Weikening tablet and application thereof
A fingerprint and Weikening tablet technology, which is applied in the field of detecting fingerprints of amino acid components in Weikening tablets and Weikening tablets
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Embodiment 1
[0109] 1. Experimental part
[0110] 1.1 Sample pretreatment
[0111] Preparation of the test solution: Accurately weigh 2 g of Wei Ke Ning Tablets, place in a 100 mL Erlenmeyer flask, add 25 mL of 6mol / L hydrochloric acid to dissolve, then place in a water bath at 100±1°C for 8 hours, take it out to cool, and take the aqueous solution Put 10mL in an evaporating dish, concentrate to dryness in a water bath at 100±1°C, add 5mL of 0.1mol / L dilute hydrochloric acid to dissolve, filter through a needle filter with a 0.45μm filter membrane, and take the clear liquid for derivatization.
[0112] 1.2 Derivatization
[0113] Accurately measure 400 μL of the test solution, place it in a 2 mL centrifuge tube, add 200 μL of acetonitrile solution of 1mol / L triethylamine and 200 μL of acetonitrile solution of 0.1mol / L phenylisothiocyanate, shake well and let stand at room temperature to derivatize 1 Hour. After derivatization, add 800 μL of n-hexane, shake and stand for 10 min, take 400...
Embodiment 2
[0132] 1. Experimental part
[0133] 1.1 Sample pretreatment
[0134] Preparation of the test solution: accurately weigh a certain amount of Wei Ke Ning tablets, place in a 100mL Erlenmeyer flask, add 5-7mol / L hydrochloric acid to dissolve, the weight of Wei Ke Ning tablets added is the same as that of 5-7mol / L hydrochloric acid The volume ratio is 1:10-15 (g / ml). Then place it in a water bath at 100±5°C for 7-9 hours and take it out to cool. Take the aqueous solution and place it in an evaporating dish, concentrate it in a water bath at 100±5°C to dryness, and add the aqueous solution to 5-7mol / L hydrochloric acid at a volume ratio of 1:2-3. Then add 0.05-0.2mol / L dilute hydrochloric acid to dissolve, and the volume ratio of 0.05-0.2mol / L dilute hydrochloric acid to 5-7mol / L hydrochloric acid is 1:1-3. After filtering with a needle filter with a 0.45 μm filter membrane, the supernatant was taken and stored in a refrigerator at 4°C for derivatization.
[0135] 1.2 Derivati...
Embodiment 3
[0153] 1. Experimental part
[0154] 1.1 Sample pretreatment
[0155] Preparation of the testing solution: same as the preparation process of the testing solution in step 1.1 in Example 1.
[0156] 1.2 Pretreatment of reference substance
[0157] Preparation of reference substance solution: Accurately weigh 20 mg of glycine, arginine, alanine, leucine and phenylalanine reference substances respectively, dissolve with 0.1mol / L hydrochloric acid and constant volume, shake well, and gradually dilute , Obtain the reference substance solution from the reference substance stock solution. The contents of glycine, arginine, alanine, leucine, and phenylalanine in the reference solution were all 100 μg / ml.
[0158] 1.3 Derivatization
[0159] The derivatization process of the test solution is the same as that of the test solution in step 1.2 of Example 1.
[0160] Accurately measure 400 μL of the reference solution in step 1.2, place it in a 2 mL centrifuge tube, add 200 μL of acet...
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