CN102253153B - Method for optimizing gradient elution condition of ion chromatographic determination of anion in tobacco leaf by response surface methodology - Google Patents
Method for optimizing gradient elution condition of ion chromatographic determination of anion in tobacco leaf by response surface methodology Download PDFInfo
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- CN102253153B CN102253153B CN201110089049.5A CN201110089049A CN102253153B CN 102253153 B CN102253153 B CN 102253153B CN 201110089049 A CN201110089049 A CN 201110089049A CN 102253153 B CN102253153 B CN 102253153B
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Abstract
The invention relates to a method for optimizing chromatographic separation conditions, and particularly relates to a method for optimizing gradient elution conditions of ion chromatographic determination of anions in tobacco leaves by response surface methodology. The invention is a method for optimizing gradient elution conditions of ion chromatographic determination of anions in tobacco leaves by response surface methodology; only 27 groups of experiments is required for the optimization of gradient leaching conditions, which shortens the analysis time, and increases the analysis efficiency; the invention can optimize the gradient optimization conditions reasonably and effectively only through a few experiments, and is simple and rapid; the invention is applicable to a series of issues for optimization of gradient elution conditions of liquid chromatography, and has quite high practical value.
Description
Technical field
The present invention relates to a kind of optimization method of chromatographic separation condition, particularly relate to the method for utilizing Response Surface Method to optimize the condition of gradient elution of negative ion in ion chromatography tobacco leaf.
Background technology
Inorganic anion and organic acid are extensively present in tobacco, the physiological metabolism in tobacco growing process is played an important role, and to Sensory Quality of Cigarette important, for example many organic acids and derivant thereof are the principal ingredients of tobacco flavor.Therefore by the analysis and research to organic acid in tobacco and inorganic ions, to judge flue gas whether alcohol and, evaluate tobacco leaf quality, instruct leaf tobacco production and tobacco leaf formulation all significant.Chromatography of ions, as efficient, simple, quick, a highly sensitive technology analyzing zwitterion, is the important method of separating organic acid molecule and inorganic ions.
In chromatography of ions field, linear gradient elution method can shorten analytical cycle, improves separating power, improves peak type and increase sensitivity.Particularly complex biological sample as the analytic process of tobacco leaf in, it is particularly important that linear gradient elution method seems.But the parameter that this method need to be optimized is more, optimize difficulty also larger.At present, response surface optimization, as the very effective chemometrics method of one, is widely used in the aspects such as sample pre-treatments, electrophoresis and mass spectrum condition optimizing.It obtains maximum relevant informations with minimum experiment number.From these information, just can find best condition of gradient elution by certain evaluation method.
Summary of the invention
The invention provides a kind of optimization method of chromatography of ions gradient elution condition, utilize a Dionex ICS-2100 ion chromatograph and AS19 ion chromatographic column to detect negative ion in tobacco leaf, use Response Surface Method to optimize gradient elution condition, can realize 12 kinds of negative ion and analyze at short notice simultaneously, greatly improve analysis efficiency.
Concrete technical scheme of the present invention is as follows:
The present invention is a kind of method that Response Surface Method is optimized the condition of gradient elution of negative ion in ion chromatography tobacco leaf, only can be optimized gradient elution condition by 27 groups of experiments, has shortened analysis time, has improved analysis efficiency.
The present invention only, by a small amount of experiment, just can optimize gradient optimizing condition rationally and effectively, easy to be quick.
The present invention goes for the problem that a series of liquid chromatography condition of gradient elution are optimized, and has very high practical value.
Tool of the present invention has the following advantages and effect:
1. the present invention utilizes Response Surface Method, only can be optimized gradient elution condition by 27 groups of experiments, has shortened analysis time, has improved analysis efficiency.
2. the present invention goes for the problem of series of optimum chromatogram gradient elution condition, has very high practical value.
brief description of the drawings
Fig. 1 is gradient condition type;
Fig. 2 is the actual sample signal peak while not optimizing chromatography of ions condition of gradient elution by Response Surface Method;
Fig. 3 is that Response Surface Method is optimized the actual sample signal peak after chromatography of ions condition of gradient elution;
In Fig. 1, be labeled as:
T
1-subordinate phase the start time, c
1-subordinate phase finishes concentration, t
2start time-phase III, c
2-the phase III finishes concentration;
In Fig. 2, be labeled as:
1-acetate, 2-formate, 3-chlorion, 4-nitrate radical, 5-sulfate radical, 6-malate, 7-oxalate, 8-phosphate radical, 9-citrate;
In Fig. 3, be labeled as:
1-acetate, 2-formate, 3-chlorion, 4-nitrate radical, 5-sulfate radical, 6-malate, 7-oxalate, 8-phosphate radical, 9-citrate.
Embodiment
The present invention utilizes Response Surface Method to optimize gradient elution condition, and gradient condition (see figure 1) is to be divided into four-stage, and the first stage, leacheate is constant; Subordinate phase, eluent concentration is linear to raise; Phase III, eluent concentration is linear to raise, and rising slope is different from subordinate phase; Fourth stage, eluent concentration is down to first stage concentration.
The factor of Response Surface Method optimization is the start time and end concentration of subordinate phase, the start time of phase III and end concentration.Utilize chromatographic response function (CRF) as response, be optimized as target to obtain the highest CRF.
The present invention utilizes Dionex ICS-2100 ion chromatograph and AS19 ion chromatographic column, the simple online leacheate of KOH, and single pump single-flow-path system, inhibition type electricity is led detection.
The gradient condition optimization method that the present invention adopts is Response Surface Method.First, rule of thumb determine gradient elution type, then utilize Response Surface Method to obtain the experimental design tables (table 1) of 27 groups of experiments, utilize chromatographic response function (CRF) as response, be optimized as target to obtain the highest CRF.
Chromatographic response function (CRF) calculating formula
(1)
(2)
Wherein, R
i, i+1for the degree of separation between adjacent two peak i and i+1, t
i, and t
i+1be respectively the retention time of peak i and i+1, w
iand w
i+1be respectively the peak width of peak i and i+1, the retention time that T is last material.
Table 1
Traditional gradient optimizing process is mainly by micro-judgment, but the parameter that need to optimize is more, optimizes difficulty also larger, and the chromatographic condition often obtaining not is optimal conditions.First, we have used traditional gradient optimizing method, rule of thumb determine gradient condition, and process is loaded down with trivial details, and result as shown in Figure 1.The gradient condition optimization method that the present invention adopts is Response Surface Method, only can be optimized gradient elution condition by 27 groups of experiments, and result as shown in Figure 2.Comparison diagram 1 and Fig. 2 are known, and the gradient condition that the Response Surface Method that the present invention adopts obtains can significantly shorten disengaging time, improves peak shape, and target substance has also obtained good separation.
The present invention adopts the ion chromatograph Dionex ICS-2100 of Dai An company of the U.S. (Dionex); Ionpac AG19 (50mm × 4mm) guard column; Ionpac AS19 (250mm × 4mm) analytical column, the KOH leacheate generator of employing Dai An company.Flow rate of mobile phase is 1.0mL/min, and sample size is 25 μ L, and after ASRS300-4mm galvanochemistry self-reproduction suppresser suppresses, DS6 electric conductivity detector detects.
Claims (1)
1. Response Surface Method is optimized a method for the condition of gradient elution of negative ion in ion chromatography tobacco leaf, it is characterized in that only can being optimized gradient elution condition by 27 groups of experiments, has shortened analysis time, has improved analysis efficiency; Wherein, the gradient condition of use is to be divided into four-stage, and the first stage, leacheate is constant; Subordinate phase, eluent concentration is linear to raise; Phase III, eluent concentration is linear to raise, and rising slope is different from subordinate phase; Fourth stage, eluent concentration is down to first stage concentration; The factor of Response Surface Method optimization is the start time and end concentration of subordinate phase, the start time of phase III and end concentration; Utilize chromatographic response function (CRF) as response, be optimized as target to obtain the highest CRF.
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| CN201110089049.5A CN102253153B (en) | 2011-04-11 | 2011-04-11 | Method for optimizing gradient elution condition of ion chromatographic determination of anion in tobacco leaf by response surface methodology |
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| CN201110089049.5A CN102253153B (en) | 2011-04-11 | 2011-04-11 | Method for optimizing gradient elution condition of ion chromatographic determination of anion in tobacco leaf by response surface methodology |
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| CN102253153B true CN102253153B (en) | 2014-06-04 |
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| CN105784908B (en) * | 2016-04-13 | 2017-10-10 | 广东中烟工业有限责任公司 | The chromatography of ions detection method of 6 kinds of anion in cigarette paper |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101773593A (en) * | 2009-12-08 | 2010-07-14 | 江苏省农业科学院 | Method for preparing antioxidative active extractive of sweet potato leaves |
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| CN101773593A (en) * | 2009-12-08 | 2010-07-14 | 江苏省农业科学院 | Method for preparing antioxidative active extractive of sweet potato leaves |
Non-Patent Citations (2)
| Title |
|---|
| 响应曲面法优选人工蛹虫草多糖微波提取工艺;宋江峰 等;《江苏农业学报》;20091231;第25卷(第5期);摘要 * |
| 宋江峰 等.响应曲面法优选人工蛹虫草多糖微波提取工艺.《江苏农业学报》.2009,第25卷(第5期),1143-1150. |
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