Method of determining low-content paricalcitol through high performance liquid chromatography-tandem mass spectrometry method and application thereof

A high-performance liquid chromatography and paricalcitol technology, which is applied in the field of analytical chemistry, can solve the problems of difficult to meet the quantitative determination of dissolution, interfere with the determination of the main peak paricalcitol, and low specifications of the main drug, and achieve accuracy. Good, sensitive and specific effects

Inactive Publication Date: 2016-03-02
CHONGQING HUAPONT PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This detection method adopts ordinary liquid chromatography, and it is difficult to meet the requirements of quantitative determination of dissolution due to the low specification of the main drug.
In addition, the dissolution medium selected by this method has a la

Method used

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  • Method of determining low-content paricalcitol through high performance liquid chromatography-tandem mass spectrometry method and application thereof
  • Method of determining low-content paricalcitol through high performance liquid chromatography-tandem mass spectrometry method and application thereof
  • Method of determining low-content paricalcitol through high performance liquid chromatography-tandem mass spectrometry method and application thereof

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Experimental program
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Embodiment 1

[0074] The research of detection limit and limit of quantification of embodiment 1 test method of the present invention

[0075] Accurately weigh 0.02516g of the Paricalcitol reference substance (content 98.6%), put it in a 250ml measuring bottle, add absolute ethanol to dissolve and dilute to the mark, shake well, and use it as the reference substance stock solution; accurately pipette an appropriate amount of this solution , taking 500ml of 0.4% lauryl dimethyl amine oxide solution (adding about 10ng / ml of dutasteride as an internal standard) as the dissolution medium, quantitatively diluting to make about 40pg and 80pg of paricalcitol per 1ml solution. According to the above-mentioned liquid chromatography-mass spectrometry conditions, 100 μl were precisely measured and injected into a liquid chromatograph, and the HPLC-MRM spectrum was recorded.

[0076] Such as image 3 and Figure 4 as shown, image 3 For paricalcitol detection limit chromatogram (its signal-to-noise...

Embodiment 2

[0077] Embodiment 2 Application of the inventive method in the dissolution determination of Paricalcitol Soft Capsules

[0078] Using the above-mentioned liquid chromatography-mass spectrometry conditions, wherein the sample solution preparation process is as follows: take 1 paricalcitol soft capsule, add 500ml of 0.4% lauryl dimethyl amine oxide solution (add about 10ng / ml of dutasteride (as an internal standard) is the dissolution medium, and the rotating speed is 100 revolutions per minute, operated according to the rotating basket method. After 20, 30, 45, and 60 minutes, take an appropriate amount of eluate, filter it with a 0.45 μm organic membrane, and take the subsequent filtrate as the sample solution. Another appropriate amount of paricalcitol reference substance stock solution was taken, and quantitatively diluted with the aforementioned same dissolution medium to make a solution containing about 4 ng of paricalcitol in every 1 ml, as the reference substance solutio...

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Abstract

The invention belongs to the technical field of analytical chemistry and particularly relates to a method of determining low-content paricalcitol through a high performance liquid chromatography-tandem mass spectrometry method and application thereof. According to the method, the high performance liquid chromatography-tandem mass spectrometry method is adopted for determination, an internal standard method is also adopted, and dutasteride is used as an internal standard substance. The method is high in specificity, sensitivity and accuracy, the detection limit of the method can reach 40 pg/ml, and the quantization limit can reach 80 pg/ml. The method can be widely applied to testing of the content and dissolution rate of a low-content paricalcitol preparation, and particularly testing of the dissolution rate of a paricalcitol soft capsule.

Description

technical field [0001] The invention aims at the technical field of analytical chemistry, and in particular relates to a method for testing low-content paricalcitol content and an application thereof. Background technique [0002] Paricalcitol is an analogue of vitamin D active substance calcitriol, which is used for the prevention and treatment of secondary hyperparathyroidism (mainly manifested as PTH elevation). Molecular formula is C 27 h 44 o 3 , the chemical name is (7E,22E)-19-desmethyl-9,10-cycloergosta-5,7,22-triene-1α,3β,25-triol, and its structural formula is as follows: [0003] [0004] The specifications of the main drug in Paricalcitol soft capsules include 1 μg / capsule, 2 μg / capsule and 4 μg / capsule, all of which are low specifications. Referring to the dissolution test method of Paricalcitol Soft Capsules in the FDA, 500ml of a solution containing 0.4% lauryl dimethylamine oxide (LADO) was used as the dissolution medium, and the final concentration of...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 管璐晗赵静陈李平
Owner CHONGQING HUAPONT PHARMA
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