CN102128886A - High performance liquid chromatography method for measuring stabilizer BHT content of tetrahydrofuran - Google Patents
High performance liquid chromatography method for measuring stabilizer BHT content of tetrahydrofuran Download PDFInfo
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- CN102128886A CN102128886A CN2010105807254A CN201010580725A CN102128886A CN 102128886 A CN102128886 A CN 102128886A CN 2010105807254 A CN2010105807254 A CN 2010105807254A CN 201010580725 A CN201010580725 A CN 201010580725A CN 102128886 A CN102128886 A CN 102128886A
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- tetrahydrofuran
- bht
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- stabilizing agent
- acetonitrile
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Abstract
The invention discloses a high performance liquid chromatography method for measuring stabilizer 2,6-ditertiary butyl-4-methyl phenol (BHT ) content of tetrahydrofuran, which comprises the following steps of: 1) setting the conditions of high performance liquid chromatography, namely a C18 inverse phase chromatographic column has a length of 5 microns and an inside diameter of 150*4.6 millimeters (I.D.), the ratio of mobile phone to methanol to acetonitrile to water is 50-70: 10-40: 10-30 (v/v), the flow rate is 1.0ml/min, the column temperature is 40 DEG C, the detection wavelength is 277 nanometers, the sampling volume is 5.0mul and the retention time is 27.0 minutes; 2) preparing stabilizer BHT standard solution; 3) making a standard curve; and 4) measuring sample content, wherein the measured lowest detection limit of the stabilizer BHT is 0.0002mg/ml. By the method, the stabilizer BHT content of the tetrahydrofuran can be accurately measured, and reliable detection data are provided for ensuring the stability of the BHT content of a tetrahydrofuran product and the quality control of the product.
Description
Technical field
The invention belongs to the analytical chemistry field, be specifically related to the HPLC analytical method of stabilizing agent BHT (2,6 di tert butyl 4 methyl phenol) content in a kind of mensuration tetrahydrofuran.
Background technology
Tetrahydrofuran (THF) is called 1 again, and 4-epoxy butane, tetrahydrofuran have characteristics such as low toxicity, low boiling, good fluidity, are a kind of important organic synthesis and fine chemical material, have purposes widely.Tetrahydrofuran can be used for making the surface conditioning agent of anticorrosive paint, printing ink, extractant, leatheret; Aspect medical, tetrahydrofuran can be used as the raw material of synthetic carbetapentane citrate, sharp pluramycin, progesterone and some hormone drugs; As the important source material of producing polymethylene glycol ether (PTMEG), tetrahydrofuran is used for synthetic thermoplastic polyurethane, copolyester ether and polyurethane elastomeric fiber (spandex), be used for the processing of synthetic resin and natural resin, tetrahydrofuran also has the excellent solvent performance, can directly be used as solvent.
In the prior art, since tetrahydrofuran can with oxygenant generation kickback, meet naked light, high heat, strong oxidizer and very easily cause combustion explosion, so, ingress of air or under illumination condition, easily generate superoxide when not adding stabilizing agent with potential explosion hazard.Usually in the production run of tetrahydrofuran, need to add antioxidant BHT or analog as stabilizing agent, but the quality and the application performance that how much directly influence product of stabiliser content, therefore need carry out detection by quantitative to the stabilizing agent in the tetrahydrofuran, guarantee that stabilizing agent keeps certain content in tetrahydrofuran.
Do not see at present the report of measuring the HPLC analytical method of stabilizing agent BHT content in the tetrahydrofuran.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of HPLC analytical method of measuring stabilizing agent BHT content in the tetrahydrofuran, to fill up in the prior art blank to stabilizing agent BHT detection by quantitative in the tetrahydrofuran.
The HPLC analytical method of stabilizing agent BHT content comprises the steps: in the mensuration tetrahydrofuran of the present invention
1) condition of high performance liquid chromatography is as follows:
Reverse-phase chromatographic column: C
18, 5 μ m, 150 * 4.6mm (I.D.),
Moving phase: methyl alcohol: acetonitrile: water=50-70: 10-40: 10-30 (v/v),
Flow velocity: 1.0ml/min,
Column temperature: 40 ℃, sample size: 5.0 μ l,
Detect wavelength: 277nm,
Stabilizing agent BHT retention time: 27.0min.
2) preparation stabilizing agent BHT standard solution is better in the organic phase dissolubility because stabilizing agent BHT is poorly soluble in water, and the present invention adopts above-mentioned moving phase dissolving and dilution preparation stabilizing agent BHT standard solution;
3) between 200-400nm, carry out continuous sweep with diode display detecting device; Formulate typical curve, measure peak area, calculate the content of stabilizing agent BHT in the sample.
Beneficial effect of the present invention:
1) adopts C
18Reverse-phase chromatographic column is accurately measured the content of stabilizing agent BHT in the tetrahydrofuran with HPLC analytical method, and uses the moving phase sample dissolution, has guaranteed the stability of solution;
2) sampling volume is 5.0 μ l, and column temperature is 40 ℃, has improved the symmetry of chromatographic peak;
3) can rapid and accurate determination the content of stabilizing agent BHT in the tetrahydrofuran, its lowest detection is limited to 0.0002mg/ml, the inventive method provides the reliable detection data for the stability of guaranteeing BHT content in the tetrahydrofuran product and the quality control of product.
Description of drawings
Fig. 1 is the ultraviolet spectrogram of stabilizing agent BHT.
Fig. 2 is the ultraviolet spectrogram of tetrahydrofuran.
Fig. 3 is a mobile phase A methyl alcohol: the chromatogram during water=50: 50 (v/v).
Fig. 4 is the Mobile phase B acetonitrile: the chromatogram during water=50: 50 (v/v).
Fig. 5 is a mobile phase methanol: acetonitrile: the chromatogram during water=60: 20: 20 (v/v).
Fig. 6 is a mobile phase methanol: acetonitrile: the chromatogram during water=60: 16: 24 (v/v).
Fig. 7 is the canonical plotting of stabilizing agent BHT.
Embodiment
The invention will be further described below by embodiment, but embodiment does not limit protection scope of the present invention.Main experimental apparatus and chromatographic condition:
Waters 1525 type high performance liquid chromatographs, Waters 717plus automatic sampler is joined Waters 2996 type diode array (PDA) detecting devices, and the control of chromatographic fractionation system and record are finished by Waters Empower chromatogram management system.
Chromatographic column is selected for use: C
18, 5 μ m, 150 * 4.6mm (I.D), mobile phase methanol: acetonitrile: water=50-70: 10-40: 10-30 (v/v), flow velocity: 1.0ml/min, column temperature: 40 ℃, detect wavelength: 277nm.
Reagent and medicine:
Stabilizing agent BHT reference substance (＞99.0wt%);
Methyl alcohol: HPLC level; Acetonitrile: HPLC level;
Sample: contain the tetrahydrofuran of stabilizing agent BHT, prepare and get through pre-treatment removal superoxide, drying, rectifying.
Moving phase and solution with water are the quartzy distilled water of secondary in the experiment.
Embodiment 1 detects the selection of wavelength
Carry out continuous sweep with diode array detector at 240-400nm, obtain uv absorption spectra (referring to Fig. 1-2).As shown in Figure 1, stabilizing agent BHT has absorption maximum near 277nm; As shown in Figure 2, tetrahydrofuran does not have maximum absorption wavelength in the 240-400nm interval, so selecting to detect wavelength is 277nm.
The selection of embodiment 2 moving phases
The moving phase of different volumes ratio formed compare shaker test, when selecting methyl alcohol and water when (v/v) was as mobile phase A in 50: 50, stabilizing agent BHT chromatographic peak can not separate at all, and its separating effect is referring to Fig. 3; When selecting acetonitrile and water to press 50: 50 (v/v) as Mobile phase B, stabilizing agent BHT chromatographic peak can not reach good separation, and conditions of streaking is serious, and its separating effect is referring to Fig. 4.
This shows that moving phase selects methanol-water, acetonitrile-water all not to have good separating effect, and according to the peak shape variation tendency, the present invention is chosen as methyl alcohol-acetonitrile-water mixed solvent with moving phase, has obtained effect preferably, the part test result is referring to table 1.
Wherein, under the volume ratio of methyl alcohol, acetonitrile, water was 60: 20: 20 conditions, each composition can reach baseline separation, conditions of streaking slightly, and separating effect is referring to Fig. 5.
Under the volume ratio of methyl alcohol, acetonitrile, water was 60: 16: 24 conditions, each composition can reach baseline separation, no conditions of streaking, and separating effect is referring to Fig. 6.
The data of table 1 moving phase contrast shaker test
| Moving phase component (v/v) | Separating effect |
| Methyl alcohol: acetonitrile: water=55: 30: 15 | Baseline separation, no conditions of streaking |
| Methyl alcohol: acetonitrile: water=60: 20: 20 | Baseline separation, conditions of streaking slightly |
| Methyl alcohol: acetonitrile: water=60: 16: 24 | Good separating effect, no conditions of streaking |
| Methyl alcohol: acetonitrile: water=64: 16: 20 | Baseline separation, no conditions of streaking |
Data according to the contrast of the moving phase in the table 1 shaker test, found that: when to select moving phase be methyl alcohol-acetonitrile-water mixed solvent, effect is preferable, and work as methyl alcohol: acetonitrile: water=50-70: 10-40: 10-30 (v/v), all can obtain separating effect preferably, wherein, the optimal flow phase component is a methyl alcohol: acetonitrile: water=60: 16: 24 (v/v).
The preparation of embodiment 3 standard solution
Accurately take by weighing 2.500mg stabilizing agent BHT standard reference material, place the 10ml volumetric flask, with moving phase dissolving and be diluted to scale, shake up, being made into concentration is the standard reserving solution of the stabilizing agent BHT of 0.25mg/ml, uses the moving phase stepwise dilution to desired concn during use.
The making of embodiment 4 typical curves
High-efficient liquid phase chromatogram condition is: reverse-phase chromatographic column is C
18, 5 μ m, 250 * 4.6mm (I.D); The volume ratio that moving phase consists of is a methyl alcohol: acetonitrile: water=60: 16: 24; Flow velocity is 1.0ml/min; Column temperature is 40 ℃; The detection wavelength is 277nm.
Get the stabilizing agent BHT standard solution 5 μ l sample introductions of above-mentioned preparation, with peak area concentration is mapped, specifically referring to Fig. 7.
As shown in Figure 7, stabilizing agent BHT is in the scope of concentration 0.1-0.6mg/ml the time, and BHT standard items concentration and peak area are linear, and equation of linear regression is: Y
BHT=7969+2 * 10
6X, r=0.9995.
When signal to noise ratio (S/N ratio) S/N=10, the lowest detection that records stabilizing agent BHT is limited to 0.0002mg/ml.
Stabilizing agent BHT Determination on content in embodiment 5 samples
High-efficient liquid phase chromatogram condition is: reverse-phase chromatographic column is C
18, 5 μ m, 250 * 4.6mm (I.D); The volume ratio that moving phase consists of is a methyl alcohol: acetonitrile: water=60: 16: 24; Flow velocity is 1.0ml/min; Column temperature is 40 ℃; The detection wavelength is 277nm.
Get the tetrahydrofuran sample 5.0 μ l direct injected that contain stabilizing agent BHT, carry out efficient liquid phase chromatographic analysis, referring to Fig. 6.
After measured, the content of stabilizing agent BHT is 0.2mg/ml in the tetrahydrofuran.
Should be noted that at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical scheme of invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (3)
1. a HPLC analytical method of measuring stabilizing agent BHT content in the tetrahydrofuran is characterized in that, comprises the steps:
1) condition of high performance liquid chromatography is:
Reverse-phase chromatographic column: C
18, 5 μ tm, 150 * 4.6mm (I.D.),
Moving phase: methyl alcohol: acetonitrile: water=50-70: 10-40: 10-30 (v/v),
Flow velocity: 1.0ml/min,
Column temperature: 40 ℃,
Detect wavelength: 277nm,
Sampling volume: 5.0 μ l,
Retention time: 27.0min;
2) preparation stabilizing agent BHT standard solution;
3) production standard curve;
4) mensuration of sample size.
2. HPLC analytical method according to claim 1 is characterized in that, described moving phase is preferred: methyl alcohol: acetonitrile: water=60: 16: 24 (v/v).
3. HPLC analytical method according to claim 1 is characterized in that, adopts moving phase dissolving and dilution preparation stabilizing agent BHT standard solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102928545A (en) * | 2012-11-09 | 2013-02-13 | 江苏吉贝尔药业有限公司 | Method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops |
-
2010
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Non-Patent Citations (5)
| Title |
|---|
| J. F. SCHABRON等: "Determination of BHT, Irganox 1076, and Irganox 1010 Antioxidant Additives in Polyethylene by High Performance Liquid Chromatography", 《ANALYTICAL CHEMISTRY》 * |
| 蔡发等: "高效液相色谱法同时测定食品中的12种抗氧化剂", 《食品科学》 * |
| 蔡玉枝等: "高效液相色谱法快速测定食品中抗氧化剂BHA、BHT", 《分析测试学报》 * |
| 薛艳等: "反相高效液相色谱-质谱法测定喷气燃料中抗氧剂含量", 《色谱》 * |
| 谢增鸿等: "《食品安全分析与检测技术》", 30 September 2010 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102928545A (en) * | 2012-11-09 | 2013-02-13 | 江苏吉贝尔药业有限公司 | Method for measuring BHT (butylated hydroxytoluene) content in Pranoprofen eye drops |
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Address after: 200072 Zhabei District, Shanghai, Shanghai Road, No. 1, building 801, No. Applicant after: Sinopharm Chemical Reagent Co., Ltd. Address before: 200333, room 26, No. 540, Lane 302-3, Daning Road, Shanghai, Zhabei District Applicant before: Sinopharm Chemical Reagent Co., Ltd. |
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