Detection method for illegally added medicine in blood fat reducing Chinese patent medicine and health food
A health food and illegally added technology, applied in the field of ultra-high performance liquid chromatography-tandem mass spectrometry, can solve the problems of weak qualitative ability, few detection components, long detection time, etc., and achieve the effect of accurate method, strong specificity and high sensitivity
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Embodiment 1
[0019] Embodiment 1: investigation verification of experimental method
[0020] (1) Chromatography-mass spectrometry conditions: Chromatographic column: Waters Acquity BEH-C 18 (2.1mm×50mm, 1.7µm);
[0021] Mobile phase: aqueous solution containing 0.05% formic acid (A) - acetonitrile (B) Gradient elution: 0~2.5min, 50%B, 2.5~3.0min, 60%B, 3.0~3.5min, 100%B, 3.5~ 4.0min, 50%B, flow rate 0.15mL / min; column temperature: 25℃; injection volume 5µL. Mass spectrometry conditions: electrospray ion source ESI positive ion mode scan; capillary voltage 2.5kV; desolvation gas temperature 450°C; desolvation gas flow rate 750L / h; cone gas flow rate 45L / h; collision gas is argon; product ion scan and MRM mode simultaneous monitoring;
[0022] Mobile phase: aqueous solution containing 0.75% formic acid (A) - acetonitrile (B) Gradient elution: 0~2.5min, 50%B, 2.5~3.0min, 60%B, 3.0~3.5min, 100%B, 3.5~ 4.0min, 50%B, flow rate 0.25mL / min; column temperature: 35℃; injection volume 0.5µL. ...
Embodiment 2
[0035] Embodiment 2: the mensuration of sample
[0036] (1) Preparation of reference solution
[0037] Lovastatin (batch number: LK10O58, content 98.0%, China Institute for Food and Drug Control), mevastatin (batch number: 2-NYL-167-1, content 98.0%, China Institute for Food and Drug Control), and Simvastatin (batch number: 11-SCC-167-1, content 98.0%, China Institute for Food and Drug Control), pravastatin sodium (batch number: 8-XJZ-27-1, content 98.0%, China Food and Drug Control Research Institute) Institute), fluvastatin sodium (batch number: 7-ABY-122-1, content 98.0%, China Institute for Food and Drug Control), niacin (batch number: LF80N66, content 99.5%, China Institute for Food and Drug Control) 1- 5mg, put in a 10mL volumetric flask, add methanol to dissolve and dilute to the volume, shake well, and use it as the standard stock solution of each standard. According to the mass spectrometry response results of the preliminary analysis, an appropriate amount of the s...
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