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Derivatization treatment method for drug enantiomer detection, determination method and application

A technology of enantiomer and determination method, applied in the field of derivatization treatment method and determination for drug enantiomer detection, can solve the problems of high cost, poor reproducibility, long preparation time of the test sample, etc. Simple operation, easy control, accurate and reliable test results

Active Publication Date: 2021-10-08
SICHUAN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a derivatization treatment method for the detection of drug enantiomers, which is used for sitagliptin phosphate bulk drug and The detection of the S-enantiomer in the preparation not only has a high degree of separation between the raw material drug and the enantiomer, but also can solve the problems of long preparation time, poor reproducibility and high cost of the test product in the existing detection technology. question

Method used

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  • Derivatization treatment method for drug enantiomer detection, determination method and application
  • Derivatization treatment method for drug enantiomer detection, determination method and application
  • Derivatization treatment method for drug enantiomer detection, determination method and application

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Embodiment 1

[0060] The method for the determination of enantiomers in sitagliptin phosphate bulk drug and preparations is detected by high performance liquid chromatography.

[0061] Instruments and reagents: efficient liquid chromatography, electronic balance, pH meter, water bath, triethylamine, phosphoric acid, acetonitrile, Marfey reagent, sodium bicarbonate, hydrochloric acid;

[0062] Chromatographic conditions:

[0063] Use octadecylsilane bonded silica gel as filler, 0.72% triethylamine aqueous solution (adjust pH value to 2.0 with phosphoric acid) as mobile phase A, acetonitrile as mobile phase B, perform gradient elution according to Table 1, and use water : Acetonitrile (50:50) is the diluent, the flow rate is 1.5ml per minute, and the detection wavelength is 340nm.

[0064] Table 1

[0065]

[0066] The specific operation process includes the following steps:

[0067] S1. Sample preparation:

[0068] Need testing solution: take need testing, dissolve and dilute with dil...

Embodiment 2

[0135] The influence of small changes in chromatographic conditions on the detection results was investigated

[0136] ①The test product spiked solution-100mg: Take the test product (batch number: 210303) (specification 100mg), grind it into powder, take about 240mg→10ml of the test product ground into powder, add the above hetero S-enantiomer Dissolve 3ml of the body stock solution, ultrasonically dissolve it with a diluent and dilute to the mark to obtain (each 1ml contains about 6mg of sitagliptin and about 30μg of the S-enantiomer).

[0137] ②The test product spiked solution-50mg: Take the test product (batch number: 210301) (specification 50mg), grind it into powder, take about 240mg→10ml of the test product ground into powder, add the above S-enantiomer 3ml of the stock solution was ultrasonically dissolved with a diluent and diluted to the mark to obtain (each 1ml contains about 6mg of sitagliptin and about 30μg of S-enantiomer).

[0138] ③Blank excipient solution-100m...

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Abstract

The invention discloses a derivatization treatment method for drug enantiomer detection, a determination method and application. When the derivatization treatment method is used for detecting isomers in sitagliptin phosphate bulk drugs and preparations, high performance liquid chromatography is adopted for detection, and chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filler, a triethylamine aqueous solution is used as a mobile phase A and acetonitrile is used as a mobile phase B for gradient elution, the flow velocity is 1.5 ml per minute, and the detection wavelength is 340 nm; and a sample is prepared by adopting a reverse phase system for dissolving, and derivatization treatment is carried out by adopting a Marfeed reagent. The sitagliptin phosphate raw material medicine and enantiomer have high separation degree, the problem that an existing detection technology is long in test sample preparation time, poor in reproducibility and high in cost can be solved, and the method has the advantages of strong specificity, strong accuracy, high precision, good durability and convenience of operation, and can effectively control the quality of bulk drugs and preparations in actual production.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a derivatization treatment method for detection of drug enantiomers, a measurement method and an application. Background technique [0002] EP10.0 and USP40 have recorded the detection methods of enantiomers in sitagliptin phosphate bulk drug and preparations, but there are still problems in actual detection, although the separation of enantiomers and main peaks is relatively good , but the chromatographic column using chiral separation is a normal phase chromatographic column coated with amylose (chromatographic column 250mm×4.6mm, 5 μm) on the surface of silica gel, and 0.1% water is added to the mobile phase in the chromatographic conditions, and for 10% water was also added to the diluent used in the preparation of the test sample. It is well known that normal-phase chiral columns cannot use water as the mobile phase, nor can they dissolve samples in water. Otherwise ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 冯舟刘瑞霖赵永龙熊尧樊娇娇
Owner SICHUAN PHARMA
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