CN102262141B - Method for detecting 3,3',4',5-tetrachloro-salicylanilide by using high performance liquid chromatograph - Google Patents
Method for detecting 3,3',4',5-tetrachloro-salicylanilide by using high performance liquid chromatograph Download PDFInfo
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- CN102262141B CN102262141B CN201110095944.8A CN201110095944A CN102262141B CN 102262141 B CN102262141 B CN 102262141B CN 201110095944 A CN201110095944 A CN 201110095944A CN 102262141 B CN102262141 B CN 102262141B
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Abstract
The invention relates to a method for detecting 3,3',4',5-tetrachloro-salicylanilide by using a high performance liquid chromatograph. The method comprises steps that: a proper amount of a sample is weighed, an appropriate solvent is adopted, and a pretreatment process is carried out upon the sample through steps of vortex mixing, centrifugation, rotary evaporation and condensation, and the like; 3,3',4',5-tetrachloro-salicylanilide is detected by using a high performance liquid chromatograph connected with a diode array detector, wherein a proportion of an organic mobile phase is configured as 75%, a proportion of an inorganic mobile phase is configured as 25%, a flow rate is configured as 0.5mL/min, a sample size is configured as 10muL, a reversed-phase chromatographic column is selected as the chromatographic column, and a maximum absorption wavelength of the diode array detector is configured as 500nm. The detection method provided by the invention has characteristics of convenient, fast, high recovery rate, and the like.
Description
Technical field
The present invention relates to a kind of 3,3 ', 4 ', 5-TCSA's detection method, particularly relate to a kind of high-efficient liquid phase chromatogram technology with connecting diode array detector to detect 3,3 ', 4 ', 5-TCSA's method.
Background technology
3,3 ', 4 ', 5-TCSA is commonly used for metabolic uncoupler, adds in sewage disposal process by activated sludge process, can effectively reduce the generation of mud.
Research is found; this material has potential carcinogenicity, teratogenesis, neurotoxicity, acute toxicity, persistence, bioaccumulation etc.; < < Canadian Environmental Protection Act > > is listed in noxious material list; the cosmetics instruction 76/768/EEC of European Union is listed in the list of cosmetics banned substance; for this reason; need to be to may exist in product 3; 3 '; 4 ', 5-TCSA carries out qualitative and quantitative detection.Yet, not yet have at present 3,3 ', 4 ', 5-TCSA's detection method.For this reason, set up a kind of 3,3 ', 4 ', 5-TCSA's detection method is imperative.
Summary of the invention
The high-efficient liquid phase chromatogram technology that the technical problem to be solved in the present invention is to propose the conventional connection diode array detector of a kind of use detects 3,3 ', 4 ', 5-TCSA's method.
The present invention solve the technical problem can be by realizing by the following technical solutions:
Comprise the following steps:
1. take appropriate sample, select methyl alcohol or acetone as solvent, utilize vortex mixed instrument to extract processing to sample, the time that extraction is processed is 3-10min;
2. utilize the sample after hydro-extractor is processed extraction to carry out separation, the separated time is 5-30min, inclines and supernatant liquor;
3. utilize Rotary Evaporators to concentrate supernatant liquor, form concentrated solution;
4. concentrated solution uses the solvent identical with extraction step to carry out constant volume, crosses 0.45um filter membrane, forms the solution to be measured after pre-treatment;
5. utilize the high performance liquid chromatograph that connects diode array detector to 3 in solution to be measured, 3 ', 4 ', 5-TCSA detects, and the ratio of the organic mobile phase of described instrument is set as to 75%, and the ratio of Inorganic mobile phase sets 25%, flow velocity is set as 0.5mL/min, sample size is set as 10uL, and chromatographic column is selected reverse-phase chromatographic column, and the maximum absorption wavelength of diode array detector is set as 500nm.
Technique effect of the present invention is:
1, the high-efficient liquid phase chromatogram technology that proposes the conventional connection diode array detector of a kind of use detects 3,3 ', 4 ', 5-TCSA's method;
2, pre-treating method is easy, quick, the recovery is high;
3, by selecting suitable chromatographic column, suitable flow velocity, mobile phase ratio and maximum absorption wavelength, can make 3,3 in sample ', 4 ', 5-TCSA obtains optimized separation.
Accompanying drawing explanation
Fig. 1 be the embodiment of the present invention 1 detect 3,3 ', 4 ', 5-TCSA's chromatogram;
Fig. 2 be the embodiment of the present invention 1 detect 3,3 ', 4 ', 5-TCSA's canonical plotting.
Embodiment
Below in conjunction with the most preferred embodiment shown in accompanying drawing, be described in further detail.
Experiment condition: high performance liquid chromatograph and diode array detector, agents useful for same is chromatographically pure.In high performance liquid chromatograph and diode array detector, organic mobile phase is methyl alcohol, and ratio is set as 75%; Inorganic phase is water, and ratio is set as 25%; Flow velocity is set as 0.5mL/min; Sample size is set as 10ul; The maximum absorption wavelength of diode array detector is set as 500nm.Computer system records chromatomap, usings the peak area of object as the response of object, and sample is analyzed.
Production standard curve: the solvent that the methyl alcohol of take is preparing standard solution, preparation 3,3 ', 4 ', 5-TCSA series standard solution, carries out high performance liquid chromatograph and diode array detector coupling (HPLC-DAD) analyzing and testing by described experiment condition.Fig. 1 is 3,3 ', 4 ', 5-TCSA's chromatogram.With general objective peak area, concentration is mapped, according to 3 of standard solution horizontal survey results, set up 3,3 ', 4 ', 5-TCSA's typical curve, as shown in Figure 2, horizontal ordinate represent 3,3 ', 4 ', the concentration of 5-TCSA standard solution, ordinate represents liquid chromatography peak area response, the funtcional relationship of gained typical curve is y=29.09x+60.767, wherein y represents liquid chromatography peak area response, x represents 3,3 ', 4 ', the concentration of 5-TCSA standard solution, its linearly dependent coefficient is R
2=0.9977, this shows that this typical curve has good linear dependence.
Apply the specific embodiment that above-mentioned test condition and typical curve do as follows:
Embodiment 1
Accurately take 1g mud sample in 50mL spiral cover centrifuge tube, add wherein 20mL solvent methanol, screw pipe lid.Centrifuge tube is placed on vortex mixed instrument and disperses mixed extraction, and extraction time is 5min.Be placed in high speed centrifugation on hydro-extractor, centrifugation time is 10min.Incline and supernatant liquor.So operation is three times, merge supernatant liquor to 100mL round-bottomed flask, by Rotary Evaporators, supernatant liquor is concentrated into 5mL left and right, form concentrated solution, concentrated solution is transferred in 10mL volumetric flask, by methanol constant volume, to scale, crosses 0.45um filter membrane, form the solution to be measured after pre-treatment, carry out HPLC-DAD test.Mud sample has been made to five parallel sample, and sample number into spectrum is respectively A-1, A-2, A-3, A-4 and A-5, and analysis result is in Table 1, and to first parallel sample (sample number into spectrum is A-1) replication 5 times, analysis result is in Table 2.By table 1, known, the relative standard deviation of Duplicate Samples (RSD) is 2.82%.By table 2, known, the relative standard deviation of reperformance test (RSD) is 0.96%.
By quantitative 3,3 ', 4 ', 5-TCSA standard solution joins in above-mentioned mud sample, selects solvent same as described above, pre-treating method and instrument condition to test.Make two mark-on content, the sample of each mark-on content is done 3 horizontal surveies and is averaged, according to actual addition and measured result, (this measured result is in deduction sample 3,3 ', 4 ', result after 5-TCSA's content), calculate the recovery of standard addition of various samples, experimental result is in Table 3.As shown in Table 3, the recovery of standard addition of sample reaches more than 85%, and between 85～110%.
In table 1 mud sample 3,3 ', 4 ', 5-TCSA's test content
The test repeatability of table 2 mud sample
The recovery of standard addition of table 3 sample
Centrifuge tube is placed on vortex mixed instrument and disperses the time of mixed extraction to be set as 3min, other conditions are with embodiment 1, the relative standard deviation < 8% of gained Duplicate Samples, the relative standard deviation < 5% of reperformance test, the recovery of standard addition of sample is between 85%-110%.
Embodiment 3
Centrifuge tube is placed on vortex mixed instrument and disperses the time of mixed extraction to be set as 10min, other conditions are with embodiment 1, the relative standard deviation < 8% of gained Duplicate Samples, the relative standard deviation < 5% of reperformance test, the recovery of standard addition of sample is between 85%-110%.
Centrifugation time is set as to 5min, other conditions are with embodiment 1, the relative standard deviation < 8% of gained Duplicate Samples, the relative standard deviation < 5% of reperformance test, the recovery of standard addition of sample is between 85%-110%.
Centrifugation time is set as to 30min, other conditions are with embodiment 1, the relative standard deviation < 8% of gained Duplicate Samples, the relative standard deviation < 5% of reperformance test, the recovery of standard addition of sample is between 85%-110%.
With acetone, make solvent, other conditions are with embodiment 1, the relative standard deviation < 8% of gained Duplicate Samples, and the relative standard deviation < 5% of reperformance test, the recovery of standard addition of sample is between 85%-110%.
The above embodiment has only expressed the preferred embodiment of the present invention, it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention, it should be noted that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention; Therefore, all equalizations of doing with the claims in the present invention scope change and modify, and all should belong to the covering scope of the claims in the present invention.
Claims (4)
1. one kind 3,3 ', 4 ', 5-TCSA's detection method, is characterized in that: comprises the following steps,
1. take appropriate sample, select methyl alcohol or acetone as solvent, utilize vortex mixed instrument to extract processing to sample, the time that extraction is processed is 3-10min;
2. utilize the sample after hydro-extractor is processed extraction to carry out separation, the separated time is 5-30min, inclines and supernatant liquor;
3. utilize Rotary Evaporators to concentrate supernatant liquor, form concentrated solution;
4. concentrated solution uses the solvent identical with extraction step to carry out constant volume, crosses 0.45um filter membrane, forms the solution to be measured after pre-treatment;
5. the high performance liquid chromatograph that utilize to connect diode array detector to 3,3 in solution to be measured ', 4 ', 5-TCSA detects, in high performance liquid chromatograph and diode array detector, organic mobile phase is methyl alcohol, ratio is set as 75%; Inorganic phase is water, and ratio is set as 25%, and flow velocity is set as 0.5mL/min, and sample size is set as 10uL, and chromatographic column is selected reverse-phase chromatographic column, and the maximum absorption wavelength of diode array detector is set as 500nm.
As claimed in claim 13,3 ', 4 ', 5-TCSA's detection method, is characterized in that: described solvent is methyl alcohol.
As claimed in claim 13,3 ', 4 ', 5-TCSA's detection method, is characterized in that: utilizing vortex mixed instrument to extract the time of processing to sample is 5min.
As claimed in claim 13,3 ', 4 ', 5-TCSA's detection method, is characterized in that: utilize the sample after hydro-extractor is processed extraction to carry out the separated time for 10min.
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| CN105911162B (en) * | 2016-04-12 | 2018-01-26 | 中国检验检疫科学研究院 | The assay method of bromo and Chlorosalicylic anilide in a kind of cosmetics |
| CN105806927B (en) * | 2016-05-10 | 2018-08-17 | 中国检验检疫科学研究院 | The ion mobility spectrometry rapid detection method of 3 kinds of bromos or Chlorosalicylic anilide in cosmetics |
| CN107664665B (en) * | 2017-08-09 | 2020-06-23 | 深圳市宇驰检测技术股份有限公司 | Detection method of 3,3 ', 4', 5-tetrachlorosalicylanilide |
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Non-Patent Citations (4)
| Title |
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| N-水杨酰苯胺分子印迹聚合物的制备及识别性能研究;于莹等;《化学工程师》;20091231(第4期);63-65 * |
| 于莹等.N-水杨酰苯胺分子印迹聚合物的制备及识别性能研究.《化学工程师》.2009,(第4期),63-65. |
| 于莹等.药物柳胺酚分子印迹聚合物的制备及识别性能研究.《化工时刊》.2009,第23卷(第6期),18-20. |
| 药物柳胺酚分子印迹聚合物的制备及识别性能研究;于莹等;《化工时刊》;20090630;第23卷(第6期);18-20 * |
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