CN102565221A - Method for measuring hydrochlorothiazide drug content by ion chromatography-ultraviolet detection method - Google Patents

Method for measuring hydrochlorothiazide drug content by ion chromatography-ultraviolet detection method Download PDF

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Publication number
CN102565221A
CN102565221A CN2011104422013A CN201110442201A CN102565221A CN 102565221 A CN102565221 A CN 102565221A CN 2011104422013 A CN2011104422013 A CN 2011104422013A CN 201110442201 A CN201110442201 A CN 201110442201A CN 102565221 A CN102565221 A CN 102565221A
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China
Prior art keywords
hydrochioro
cation exchange
leacheate
detection
hydrochlorothiazide
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CN2011104422013A
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Chinese (zh)
Inventor
周丹
刘玉秀
朱岩
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Zhejiang University ZJU
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Zhejiang University ZJU
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Priority to CN2011104422013A priority Critical patent/CN102565221A/en
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Abstract

The invention provides a novel method for detecting hydrochlorothiazide. According to the novel method, an ion chromatography cation exchange system and an ultraviolet detector are combined for use, an appropriate separation condition is selected according to the difference of retention behaviors of a substance on a chromatographic column, optimal ultraviolet detection wavelength is selected, and the hydrochlorothiazide can be separated and detected under higher sensitivity. The novel method for detecting the hydrochlorothiazide can be used for detection of the content of the hydrochlorothiazide in hydrochlorothiazide drugs, pharmacodynamic research of human body fluids, and the like.

Description

Chromatography of ions-uv detection method is measured the Hydrochioro medicament contg
Technical field
The present invention relates to the using system that a kind of chemical apparatuses is analyzed, particularly relate to the chromatography of ions-ultraviolet detection system that detects Hydrochioro.
Background technology
It is a kind of in the drug for hypertension that Hydrochioro belongs to angiotensin converting enzyme inhibitor (ACEI); Commonly used have captopril, Hydrochioro, enalapril, fosinopril, Benazepril, Cilazapril, Perindopril, lisinopril and a Trandolapril etc.; The maximum persons of spinoff are captopril, nonspecific spinoff as feel sick, nervous system spinoffs such as digestive tract reaction, headache, dizziness such as vomiting.Common analytical approach mainly is that RP-HPLC separates uv detection method.Need regulate the moving phase pH value when separating about 3 with RP-HPLC, and silicagel column can not strong alkali-acid resistance and the Hydrochioro structure in contain amino, under sour environment, exist with the organic cations form, be more suitable for using ion chromatographic separation.Up to now, do not see the report of chromatography of ions-uv detection method mensuration Hydrochioro medicament contg.
Summary of the invention
The present invention to the weak point of prior art, provides a kind of chromatography of ions-cation exchange-UV-detector system just, can separation detection captopril medicine under the isocratic condition, and favorable reproducibility, highly sensitive.
The present invention is the method that a kind of chromatography of ions-uv detection method is measured the Hydrochioro medicament contg, earlier it is transformed into ionic compound through acid moving phase, separates through cation exchange column again, selects suitable wavelengths to detect.
The present invention utilizes the effect of Hydrochioro sample acid in leacheate to form down kation, is transported to guard column, cation exchange column with leacheate by pump behind the six-way valve sample introduction, passes through the separating spectrum that UV-detector obtains sample again.The separating mechanism of the method is a cation exchange, selects suitable separation conditions such as leacheate that it is well separated on cation exchange column, and selects best detection wavelength, thereby accurately measure the content of Hydrochioro.
Hydrochioro of the present invention can be able to separation detection effectively through chromatography of ions-cation exchange column, and pre-treatment is simple, and analysis time is short, highly sensitive.
The present invention also can be applied to fields such as pharmacy, pharmacokinetic study.
Beneficial effect of the present invention is following:
Do not report the method for this kind detection Hydrochioro both at home and abroad as yet; This method can be widely used in fields such as bio-pharmaceuticals, pharmacokinetic study, drug safety, food security; Can separation detection Hydrochioro medicine under the isocratic condition, favorable reproducibility, highly sensitive.
Description of drawings
Fig. 1 is the works synoptic diagram that chromatography of ions of the present invention-uv detection method is measured the Hydrochioro medicament contg;
Among the figure, the 1-leacheate; The 2-pump; The 3-six-way valve; The 4-protection is lived; The 5-cation exchange column; The 6-UV-detector; The 7-sample;
Fig. 2 is the separating spectrums of Hydrochioro standard items on cation exchange column;
Among the figure, the 1-Hydrochioro;
Fig. 3 is the separating spectrum of Kai Fute compound medicine composition on cation exchange column;
Among the figure, the 1-captopril; The 2-Hydrochioro.
Embodiment
Through specific embodiment technical scheme of the present invention is further specified below:
Chromatography of ions-uv detection method is measured the content of Hydrochioro in the Kai Fute sheet
1, the preparation of standard solution: accurately take by weighing Hydrochioro standard specimen 10mg, put adding 50% acetonitrile in the 10ml volumetric flask, after the concussion dissolving, constant volume is to scale;
2, the making of typical curve: the method preparation variable concentrations standard solution that adopts stepwise dilution;
3, sample pre-treatments: remove the tablet dressing, grind into powder accurately adds the dissolving of 50% acetonitrile after the weighing, and ultrasonic 15 minutes to be cooled to room temperature, quantitatively to scale mark.After being diluted to suitable concn, 0.45 μ m membrane filtration;
4, the selection of leacheate: test different leacheate proportionings, finally confirm as: 30% acetonitrile+5%50mM Loprazolam+65% water is separation of hydrogen chlorothiazide medicine well;
5, sample size 7 μ L, UV scanning confirms that the optimal detection wavelength is 215nm; In 0.5 μ g/ml-25 μ g/ml scope internal linear relation good (r=0.9999), detect and be limited to 0.0165 μ g/ml.
As shown in Figure 1, this method is to utilize the effect of Hydrochioro sample acid in leacheate 1 to form down kation, is transported to guard column 4, cation exchange column 5 with leacheate 1 by pump 2 behind six-way valve 3 sample introductions, passes through the separating spectrum that UV-detector 6 obtains sample again.The separating mechanism of the method is a cation exchange, selects suitable leacheate 1 condition such as separation such as grade that it is well left on cation exchange column 5, and selects best detection wavelength, thereby accurately measures the content of Hydrochioro.This method can be widely used in fields such as bio-pharmaceuticals, pharmacokinetic study, food security.
As shown in Figure 21 is 5ppm Hydrochioro standard items separating spectrums under the moving phase condition of 30% acetonitrile+5%50mM Loprazolam+65% water.
Kai Fute is a kind of compound antihypertensive medicine that contains Hydrochioro and two kinds of compositions of captopril; Be illustrated in figure 3 as through grinding; Extraction; Kai Fute sample after the dilution is separating spectrum under the moving phase condition of 30% acetonitrile+5%50mM Loprazolam+65% water, and 1 is captopril, and 2 is Hydrochioro.Hydrochioro peak type symmetry in the medicine and good with the degree of separation of captopril.

Claims (4)

1. the method for chromatography of ions-uv detection method mensuration Hydrochioro medicament contg is characterized in that, earlier it is transformed into ionic compound through acid stream leacheate (1), separates through cation exchange column (5) again, and the selection suitable wavelengths detects.
2. method according to claim 1; It is characterized in that; The effect that utilizes the acid in leacheate (1) of Hydrochioro sample is the formation kation down, is transported to guard column (4), cation exchange column (5) with leacheate (1) by pump (2) behind six-way valve (3) sample introduction, passes through the separating spectrum that UV-detector (6) obtains sample again; This separating mechanism is a cation exchange; Select suitable leacheate separation conditions such as (1) that it is gone up well at cation exchange column (5) and separate, and select best detection wavelength, thereby accurately measure the content of Hydrochioro.
3. the purposes of the method for chromatography of ions-uv detection method detection Hydrochioro medicament contg is characterized in that Hydrochioro can be able to separation detection effectively through chromatography of ions-cation exchange column, and pre-treatment is simple, and analysis time is short, highly sensitive.
4. purposes according to claim 3 is characterized in that this method also can be applied to fields such as pharmacy, pharmacokinetic study.
CN2011104422013A 2011-12-26 2011-12-26 Method for measuring hydrochlorothiazide drug content by ion chromatography-ultraviolet detection method Pending CN102565221A (en)

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Application Number Priority Date Filing Date Title
CN2011104422013A CN102565221A (en) 2011-12-26 2011-12-26 Method for measuring hydrochlorothiazide drug content by ion chromatography-ultraviolet detection method

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Citations (8)

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CN102109502A (en) * 2009-12-28 2011-06-29 扬子江药业集团上海海尼药业有限公司 Method for simultaneously detecting main component contents of quinapril hydrochloride and hydrochlorothiazide composition
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CN1654951A (en) * 2004-02-11 2005-08-17 上海市中药研究所 Quality control method for rare chrysanthemum antihypertension tablet
CN1707269A (en) * 2004-06-11 2005-12-14 上海实业联合集团药业有限公司 Method for controlling quality of zhenju hypotension preparation
US20080008751A1 (en) * 2006-07-10 2008-01-10 Michael Fox Stable formulation comprising a combination of a moisture sensitive drug and a second drug and manufacturing procedure thereof
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CN101609070A (en) * 2008-06-16 2009-12-23 北京德众万全药物技术开发有限公司 A kind of method of measuring related substances of losastan potassium/hydrochlorothiazide tablets with HPLC
CN102100743A (en) * 2009-12-16 2011-06-22 天津中新药业集团股份有限公司隆顺榕制药厂 Quality control method for hypotensive pathogenic wind dispelling tablets
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Application publication date: 20120711