CN102128883B - High performance liquid chromatography method for o-chlorocyclohexanol - Google Patents
High performance liquid chromatography method for o-chlorocyclohexanol Download PDFInfo
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Abstract
The invention discloses a high performance liquid chromatography method for o-chlorocyclohexanol, which comprises the following steps of: (1) selecting a bonded stationary phase chromatographic column; (2) selecting a mobile phase, namely organic polar reagent or water or mixture of organic polar reagent and water; (3) regulating the pH value of the mobile phone by using an inorganic acid, wherein the pH range is 1.0 to 10.0; (4) preparing o-chlorocyclohexanol standard solution and sample solution, and performing ultrasonic degassing; (5) injecting the o-chlorocyclohexanol standard solution into a liquid chromatograph, and measuring the correction factor of the o-chlorocyclohexanol; (6) injecting the o-chlorocyclohexanol sample solution into the liquid chromatograph; and (7) measuring the sample, and calculating the o-chlorocyclohexanol content of the sample. By the method, the o-chlorocyclohexanol content can be directly measured without eliminating interference, the operation is simple, a result is accurate, good reproducibility is obtained and sensitivity is high.
Description
Technical field
The present invention relates to a kind of HPLC analytical method of chlorocyclohexanol.
Background technology
Chlorocyclohexanol has another name called the 2-chloro cyclohexanol, is a kind of organic synthesis intermediate; Can add the hydrochloric acid ring-opening reaction 7-oxa-bicyclo[4.1.0 is prepared from; Also can be by cyclohexene and hypochlorous acid formulations prepared from solutions, the field of using is organic synthesis intermediate, can be used for synthetic low toxicity efficient miticide propargite.The content assaying method of chlorocyclohexanol mainly is chemical titration and vapor-phase chromatography both at home and abroad at present, and chemical titration divides direct titrimetric method and indirect titration.The chemical titration disturbing factor is more; And difficulty or ease are eliminated; Vapor-phase chromatography only is applicable to the mensuration of low content chlorocyclohexanol; Need carry out dissolution process for the high content of solid sample, cause analysis result accuracy to descend, also can't directly accurately measure for the chlorocyclohexanol vapor-phase chromatography of aqueous specimen or aqueous phase in addition.In sum, for the development that cooperates chlorocyclohexanol to use, the present invention has carried out a kind of research of HPLC analytical method of chlorocyclohexanol.
The present invention all need not special processing for no matter being the chlorocyclohexanol sample in the miscible homogeneous phase of chlorocyclohexanol or the chlorocyclohexanol of aqueous phase or organic phase and water in the organic phase, only needs get final product with the moving phase dilution after the accurate weighing.
The present invention seeks to realize like this:
(1) selects a kind of bonded stationary phase chromatographic column (preferred C30, C18, C8 or C4 post, more preferably C18) for use; Column length is 1 ~ 1000 mm (preferred 100 ~ 400 mm); Column internal diameter is 0.1 ~ 50 mm (preferred 3.0 ~ 5.0 mm); The chromatographic column filler particle size range is at 0.1 ~ 20 μ m (preferred 5.0 μ m); Detecting device is the variable wavelength UV-detector, and detecting wavelength is 100 ~ 400 nm (preferred 190 ~ 280 nm); Flow rate of mobile phase: 0.5 ~ 2.0 mL/min (preferred 0.8 ~ 1.5 mL/min).
(2) moving phase is characterized in that by the potpourri that is a kind of polar organic reagent or water or a kind of polar organic reagent and water: said polar organic reagent is a kind of (particular methanol or the acetonitrile) that is selected from methyl alcohol, acetonitrile, tetrahydrofuran, dioxane, ethanol, isopropyl alcohol, monoethylene glycol, the acetone; The volume ratio of polar organic reagent and water is 0 to 100 (preferred 95:5 to 90:10) in the moving phase.
(3) the pH value of moving phase is regulated by a kind of mineral acid, it is characterized in that: mineral acid is to be selected from perchloric acid, sulfuric acid, hydrochloric acid or phosphoric acid (preferred perchloric acid); The pH scope is 1.0 ~ 10.0 (preferred 1.8 ~ 3.5).
(4) preparation chlorocyclohexanol standard solution and sample solution, ultrasonic degas.
(5) inject the chlorocyclohexanol standard solution to liquid chromatograph, measure the correction factor of chlorocyclohexanol.
(6) inject the chlorocyclohexanol sample solution to liquid chromatograph.
(7) working sample, external standard method, internal standard method or interior additional calculation go out chlorocyclohexanol content in the sample.
Good effect of the present invention is: need not get rid of and disturb and directly measure chlorocyclohexanol content; The mensuration that both can be used for the chlorocyclohexanol of aqueous phase also can be used for the mensuration of organic phase chlorocyclohexanol, can also be used for the mensuration of the miscible homogeneous phase chlorocyclohexanol of inorganic phase and organic phase; Simple to operate, the result is accurate, and favorable reproducibility is highly sensitive.
Embodiment
Below in conjunction with embodiment the present invention is described further, but these embodiment must not be used to explain the restriction of protection domain of the present invention.
The used instrument of each embodiment is Tianjin, island LC-10A high performance liquid chromatograph; The chlorocyclohexanol standard items are self-control, content >=99.8%.
Embodiment 1
Under selected chromatographic condition: the variable wavelength UV-detector, ODS chromatographic column 5.0 μ m 250 mm * 4.6 mm (I.D.), moving phase: methyl alcohol: water=95:5 transfers to pH=2.5 with perchloric acid, detects wavelength: 210 nm, flow velocity: 1.0 mL/min.Accurately take by weighing standard items chlorocyclohexanol 0.1998 g in 50 mL volumetric flasks, be diluted to scale with moving phase.Take by weighing 2.3026 g samples in 50 mL volumetric flasks, be diluted to scale, ultrasonic degas 5 minutes with moving phase.Get standard specimen and carry out liquid-phase chromatographic analysis, sample size is 20 μ L, measures the correction factor of chlorocyclohexanol.Sample thief carries out liquid-phase chromatographic analysis, and sample size is 20 μ L, detects.Use internal standard method to calculate that chlorocyclohexanol content is 5.67% in the sample.
With adding the standard items chlorocyclohexanol in the above-mentioned sample solution; By above-mentioned experiment condition; This sample is made four mark-on content, and each mark-on content is done 3 replicate determinations and is averaged, like following table; According to actual addition and measured result, the recovery of standard addition that calculates this sample is between 99%～102%.
Embodiment 2
Under selected chromatographic condition: the variable wavelength UV-detector, ODS chromatographic column 5.0 μ m 250 mm * 4.6 mm (I.D.), moving phase: methyl alcohol: water=95:5 transfers to pH=2.5 with perchloric acid, detects wavelength: 210 nm, flow velocity: 1.0 mL/min.The mensuration of aqueous phase chlorocyclohexanol.Accurately take by weighing standard items chlorocyclohexanol 0.1005 g in 50 mL volumetric flasks, be diluted to scale with moving phase.Take by weighing 5.1967 g samples in 50 mL volumetric flasks, be diluted to scale, ultrasonic degas 5 minutes with moving phase.Get standard specimen and carry out liquid-phase chromatographic analysis, sample size is 20 μ L, measures the correction factor of chlorocyclohexanol.Sample thief carries out liquid-phase chromatographic analysis, and sample size is 20 μ L, detects.Use external standard method to calculate that chlorocyclohexanol content is 0.29% in the sample.
Embodiment 3
With 100 times of the sample solution for preparing of embodiment 2 dilutions, under the step and experiment condition identical with embodiment 2, recording the result is 0.29%, the same with routine 2 result.The detectability of method reaches 1 μ g/ml.
Embodiment 4
Under selected chromatographic condition: the variable wavelength UV-detector; ODS chromatographic column 5.0 μ m 150 mm * 4.6 mm (I.D.) moving phase: methyl alcohol: water=90:10 transfers to pH=2.0 with perchloric acid and detects wavelength: 190 nm flow velocitys: 0.8 mL/min, the mensuration of chlorocyclohexanol in the homogeneous phase.Accurately take by weighing standard items chlorocyclohexanol 0.1238 g in 50 mL volumetric flasks, be diluted to scale with moving phase.Take by weighing 2.5892 g samples in 50 mL volumetric flasks, be diluted to scale, ultrasonic degas 5 minutes with moving phase.Get standard specimen and carry out liquid-phase chromatographic analysis, sample size is 20 μ L, measures the correction factor of chlorocyclohexanol.Sample thief carries out liquid-phase chromatographic analysis, and sample size is 20 μ L, detects.Calculate through external standard method that chlorocyclohexanol content is 0.58% in the sample.
Claims (2)
1. the HPLC analytical method of a chlorocyclohexanol is characterized in that comprising the steps:
(1) select a kind of bonded stationary phase chromatographic column for use, 5.0 μ m, 250 mm * 4.6 mm ODS chromatographic columns, detecting device is the variable wavelength UV-detector, and detecting wavelength is 190 ~ 210 nm, and flow rate of mobile phase is 0.5 ~ 2.0 mL/min;
(2) moving phase is: the potpourri of first alcohol and water, and wherein, the volume ratio of first alcohol and water is methyl alcohol: water=(95-90): (5-10);
(3) the pH value of moving phase transfers to 2.0 ~ 2.5 by perchloric acid, sulfuric acid, hydrochloric acid or phosphoric acid;
(4) preparation chlorocyclohexanol standard solution and sample solution, ultrasonic degas;
(5) inject the chlorocyclohexanol standard solution to liquid chromatograph, measure the correction factor of chlorocyclohexanol;
(6) inject the chlorocyclohexanol sample solution to liquid chromatograph;
(7) working sample calculates sample chlorocyclohexanol content.
2. the HPLC analytical method of chlorocyclohexanol according to claim 1 is characterized in that adopting external standard method, internal standard method or interior additional calculation to go out chlorocyclohexanol content in the sample.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1190532A (en) * | 1998-04-02 | 1998-08-19 | 北京市诚实诚信商贸有限公司 | Method for preparing acaricide Kemante |
| CN101516878A (en) * | 2006-09-13 | 2009-08-26 | 住友化学株式会社 | Thiadiazole compound and use thereof |
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| IL154418A0 (en) * | 2000-09-19 | 2003-09-17 | Sumitomo Chemical Co | Pyrimidine compounds and their use |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190532A (en) * | 1998-04-02 | 1998-08-19 | 北京市诚实诚信商贸有限公司 | Method for preparing acaricide Kemante |
| CN101516878A (en) * | 2006-09-13 | 2009-08-26 | 住友化学株式会社 | Thiadiazole compound and use thereof |
Non-Patent Citations (5)
| Title |
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| 40%克螨特乳油的反相高效液相色谱测定;魏 翔;《河南化工》;20050831;第22卷(第8期);42-43 * |
| 周志纯.高效液相色谱法测定克螨特.《精细化工中间体》.2001,第31卷(第2期), |
| 姜欣，侯春青.反相高效液相色谱法分析克螨特.《农药》.2000,第39卷(第9期), * |
| 高效液相色谱法测定克螨特;周志纯;《精细化工中间体》;20010430;第31卷(第2期);49-50 * |
| 魏 翔.40%克螨特乳油的反相高效液相色谱测定.《河南化工》.2005,第22卷(第8期), |
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