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A kind of technology of nortadalafil and hydroxypropyl, applied in the field of detection
Inactive Publication Date: 2019-02-26
广西东盟食品药品安全检验检测中心
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[0004] In order to solve the above-mentioned technical problems in the detection of other non-drugs, the present invention provides a detection method for 2-hydroxypropyl nortadalafil, the steps are easy to operate, the specificity is strong, the sensitivity is high, and the detection efficiency is greatly improved.
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Embodiment 1
[0051] The detection method of 2-hydroxypropyl nortadalafil comprises the following steps:
[0052] (1) Preparation of the test product:
[0053] Crush and mix oyster protein powder (3g / bag), take 1g into a 50mL conical flask with a stopper, accurately add 50mL of pure methanol to weigh, ultrasonically extract for 10min, place at room temperature, weigh again, and make up for the loss with pure methanol Shake well, filter with a 0.22μm organic phase filter, take the subsequent filtrate, add methanol to dilute, the concentration is 2ng / mL, 5ng / mL, 10ng / mL, 20ng / mL, 50ng / mL, 100ng / mL, 200ng / mL, ready-to-use; see Table 3 for the linear regression equation, correlation coefficient and detection limit;
[0054] (2) Blank solution:
[0055] No sample was prepared and treated in the same way as the test sample to prepare a blank solution;
[0056] (3) Standard working curve solution preparation:
[0057] Pipette 0.010mL, 0.025mL, 0.050mL, 0.100mL, 0.250mL, 0.500mL, 1.00mL of the st...
Embodiment 2
[0063] The detection method of 2-hydroxypropyl nortadalafil comprises the following steps:
[0064] (1) Preparation of the test product:
[0065] Take 1.0mL aphrodisiac wine in a 50ml volumetric flask, add 40mL of methanol, ultrasonically extract for 10min, let it stand at room temperature, dilute to the mark with methanol, shake well, filter with a 0.22μm organic phase filter membrane, take the subsequent filtrate, add methanol to dilute , the concentration is 2ng / mL, 5ng / mL, 10ng / mL, 20ng / mL, 50ng / mL, 100ng / mL, 200ng / mL ready to use, linear regression equation, correlation coefficient and detection limit are shown in Table 3;
[0066] (2) Blank solution:
[0067] No sample was prepared and treated in the same way as the test sample to prepare a blank solution;
[0068] (3) Standard working curve solution preparation:
[0069] Pipette 0.010mL, 0.025mL, 0.050mL, 0.100mL, 0.250mL, 0.500mL, and 1.00mL of standard solutions with a concentration of 5 μg / mL 2-hydroxypropyl norta...
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Abstract
The invention discloses a detection method for 2-hydroxypropyl nortadalafil, wherein the method comprises the following steps: (1) preparation of a test sample: taking a sample, carrying out ultrasonic extraction for 10 min, adding methanol to make up the lost weight, shaking evenly, filtering with an organic phase type filter membrane, taking subsequent filtrate, and diluting for standby application; (2) preparation of a blank solution: treating without addition of the sample and according to the same method for preparing the test sample, and preparing the blank solution; (3) preparation of standard working curve solutions: taking standard solutions, adding negative sample blank matrix extract solutions, making the volume constant, and shaking evenly to be used as a series of standard working solutions for standby application; and (4) high performance liquid chromatography-tandem mass spectrometry detection: detecting a liquid chromatography tandem mass spectrometry in a positive ionmode of an ESI source, collecting by a multi-reaction monitoring (MRM) way, and quantifying by an external standard method. The pretreatment steps of the detection method are simple to operate, the detection process has strong specificity and high sensitivity, and the detection efficiency is greatly improved.
Description
technical field [0001] The invention relates to the technical field of detection, in particular to a detection method of 2-hydroxypropyl nortadalafil. Background technique [0002] The laws and regulations of our country strictly prohibit the addition of chemical substances other than food additives in food, and have always severely cracked down on such illegal additions. Under the high-pressure attack, criminals took opportunistic measures and added other analogues beyond the detection range of the current standard, such as 2-hydroxypropyl nortadalafil, which is a new type of tadalafil derivative. It has not been approved for marketing in my country, and there are no specific testing standards at home and abroad. 2-Hydroxypropyl nortadalafil uses tadalafil as the core and replaces methyl with 2-hydroxypropyl tadalafil Derivatives, these derivatives have the same core as the PDE-5 inhibitors that have been approved for marketing, and the structural differences are small. PDE...
Claims
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