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Quantitative analysis method for tadalafil in human blood plasma

A technique for quantitative analysis of tadalafil, applied in the field of biological analysis, can solve problems such as low analyte concentration, difficulty in obtaining samples, and large matrix interference, and achieve high repeatability, improved detection sensitivity, and high degree of instrument automation Effect

Pending Publication Date: 2018-10-09
武汉宏韧生物医药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The composition of tadalafil biological samples is complex, the matrix interferes greatly, and the samples are difficult to obtain and the amount is small, and the concentration of the analyte is usually very low. Therefore, the requirements for the separation and analysis technology of biological samples are getting higher and higher, and it is urgent to establish A highly sensitive and highly selective method for analyzing the content of tadalafil

Method used

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  • Quantitative analysis method for tadalafil in human blood plasma
  • Quantitative analysis method for tadalafil in human blood plasma
  • Quantitative analysis method for tadalafil in human blood plasma

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation of embodiment 1 experimental solution and working solution

[0035] Mobile phase A [referred to as MPA]: Add 1.00 mL of formic acid and about 631 mg of ammonium formate into a glass bottle filled with 1000 mL of ultrapure water, shake and mix to make an aqueous solution containing 0.1% formic acid and 10 mM ammonium formate. Storage conditions: room temperature. Validity period: 2 weeks.

[0036] Mobile phase B [referred to as MPB]: add 1.00mL of formic acid into a glass bottle containing 1000mL of acetonitrile, shake and mix to make a chromatographic grade acetonitrile solution. Storage conditions: room temperature. Validity period: 2 weeks.

[0037] Methanol: water (50:50, v:v) [denoted as R01]: add 500mL methanol and 500mL water into a glass bottle, shake and mix. Storage conditions: room temperature. Validity period: 1 month.

[0038] Methanol: dimethyl sulfoxide (9:1, v:v) [denoted as R02]: Add 18.0mL methanol and 2.00mL dimethyl sulfoxide int...

Embodiment 2

[0058] A kind of LC-MS / MS quantitative analysis method of tadalafil in human plasma, comprises the steps:

[0059] (1) Preparation of standard working solution: the gradient concentrations of tadalafil working solution were 40.0, 80.0, 400, 1600, 4000, 20000, 36000, 40000ng·mL -1 , the concentration gradient of tadalafil parallel working solution is 40.0, 120, 1800, 30000, 320000ng·mL -1 ;The gradient concentrations of calibration standards are 2.00, 4.00, 20.0, 80.0, 200, 1000, 1800, 2000ng·mL -1 , the concentrations of quality control samples were 2.00, 6.00, 90.0, 1500, 16000ng·mL -1 ;

[0060] Internal standard working solution is 400ng·mL -1 ;Accuracy / stability evaluation solution DIS is 20.0ng·mL -1 , SC1 is 2000ng·mL -1 , SC2 is 20.0ng·mL -1 ;

[0061] The preparation of the above solution only needs to ensure the final concentration, and its preparation method can be based on the preparation method of each solution in Example 1, or can be other methods.

[0062...

Embodiment 3

[0103] This example evaluates the accuracy and precision of the LC-MS / MS method in Example 2 for determining the concentration of tadalafil in human plasma. Take 20.0 μL of the quality control samples of the above four concentrations of QC-2, QC-6, QC-90, and QC-1500, and operate according to the above method, repeat the measurement 3 times for each concentration of 3 samples within 1 day, and Three analysis batches were continuously measured on different days, and the precision was calculated. The results are shown in the following table:

[0104] Analytical batch

[0105] The content LC-MS / MS detection method of tadalafil in the human plasma sample established by the present invention has an extraction recovery rate of more than 75%; the matrix effect is reduced, and the absolute matrix factor reaches between 0.85 and 1.15; the selectivity is enhanced , to reduce the interference on the quantitative analysis of analytes and internal standards; the detection is effi...

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Abstract

The invention discloses a quantitative analysis method for tadalafil in human blood plasma. The quantitative analysis method comprises: (1) preparation of a standard working solution; (2) sample treatment; (3) production of a standard curve; and (4) quantitative analysis, wherein a test sample is treated according to the step (3), and calculating is performed according to the standard curve equation obtained in the step (3) to obtain the concentration of tadalafil in the test sample. According to the present invention, the concentration of tadalafil in the human blood plasma is determined by using the liquid chromatography-mass spectrometry (HPLC-MS / MS) technology, such that the concentration of tadalafil in the human blood plasma is accurately quantitated; the chromatographic column, thedissolving liquid, the mobile phase, the mass spectrometry conditions and the like are reasonably selected, and the flow rate, the elution mode, the mass spectrometry conditions and other process conditions are optimized, such that the advantages of simple operation, high repeatability, good accuracy and high operability can be achieved; and the method can be directly used for the sample detectionanalysis in bioequivalence.

Description

technical field [0001] The invention belongs to the field of biological analysis, and more specifically relates to a method for quantitatively analyzing tadalafil in human plasma by using liquid mass spectrometry (HPLC-MS / MS). Background technique [0002] It is estimated that there are more than 150 million erectile dysfunction (ED) patients worldwide, and as the global population ages, the number of ED patients will continue to rise. Tadalafil is a selective reversible inhibitor of cyclic guanosine monophosphate (cGMP)-specific phosphodiesterase 5 (PDE5). Increased levels of cGMP in the cavernosum result in smooth muscle relaxation and blood flow into the penile tissue, producing an erection, as in asexual stimulation. At the end of 2013, Eli Lilly launched Cialis (tadalafil) in a once-daily 5mg small-dose oral dosage form in China. The strong demand in China's generic drug market, and the demand for cheap, effective and high-quality drugs can reduce the economic burden....

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 姜宏梁张杨
Owner 武汉宏韧生物医药股份有限公司
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