CN114324684A - Method for analyzing epoxypropane in sudden pollution accident - Google Patents
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Abstract
The invention discloses an analysis method of propylene oxide in sudden pollution accidents, which relates to the technical field of gas chromatography/mass spectrometry and detection, and is characterized in that a static headspace and vehicle-mounted gas chromatography/mass spectrometry combined technology is adopted to carry out on-site rapid and accurate quantitative detection and analysis on propylene oxide in sudden water pollution accidents, the static headspace is taken as a pretreatment means, experimental water is taken as a solvent, an internal standard method is adopted for quantitative analysis, and the propylene oxide and internal standard fluorobenzene are separated on a DB-624LTM medium polarity chromatographic column; the method for analyzing the propylene oxide in the sudden pollution accident has the characteristics of high temperature rising and falling speed, good anti-seismic effect, strong mobility, high sample analysis speed and the like, and is suitable for field emergency monitoring of the sudden pollution accident; according to the method for analyzing the propylene oxide in the sudden pollution accident, the interference of inert gases such as argon and carbon dioxide to the propylene oxide is avoided by adopting an MS SIM scanning mode.
Description
Technical Field
The invention relates to the technical field of gas chromatography/mass spectrometry analysis and detection, in particular to a method for analyzing epoxypropane in a sudden pollution accident, and particularly relates to a method for quickly, qualitatively and quantitatively analyzing epoxypropane for samples in environments such as water and soil of the sudden pollution accident by using a static headspace and vehicle-mounted gas chromatography/mass spectrometry.
Background
The epoxypropane is an epoxy compound with the annual output of the first 3 th place in China, is an important chemical raw material and is widely applied to the industries of polyether polyol production, pharmacy, printing and dyeing and the like. Propylene oxide is a volatile, low-boiling, flammable and explosive chemical, is confirmed by international cancer research institutes as a suspected human carcinogen, has irritation to mucous membranes and skin, can damage the cornea and conjunctiva of the eye, and causes pain in the respiratory system, skin burns and swelling, and even tissue necrosis. The method for rapidly, qualitatively and quantitatively determining the propylene oxide on site can accurately judge the property, the pollution degree, the pollution range, the environmental hazard, the water flow diffusion direction and the trend of pollutants, and better provides technical support for site treatment and pollution prevention and control of pollution accidents.
At present, the domestic and foreign monitoring methods for propylene oxide mainly concentrate on soil, sediment, air, food packaging, cosmetics and the like, and mainly comprise a gas chromatography, a portable gas chromatography, a headspace-gas method and a purging and trapping GC-MS (gas chromatography-mass spectrometry) determination method 5 analysis means. Common pretreatment means for volatile organic compounds include blowing capture and headspace, and due to low boiling point, volatility and large polarity of the propylene oxide, a target component is difficult to capture by using a blowing capture tube, so that the target component cannot be quantitatively analyzed. In addition, unknown high-concentration water sample media in sudden pollution accidents are complex and easily pollute the blowing and collecting pipe and the blowing and sweeping pipeline, and cause interference on accurate quantitative analysis of subsequent samples. In addition, the recovery rate of blowing and trapping is low, and the headspace is suitable for pretreatment analysis of samples with large polarity and unknown concentration in administrative law enforcement, petition, mass reporting and sudden pollution accidents.
On the other hand, the propylene oxide has low boiling point, is easy to volatilize and has large polarity, so the monitoring difficulty is large. Therefore, it is very important to find a simple, environment-friendly and movable on-site measuring method with strong applicability, high accuracy and good sensitivity.
Disclosure of Invention
The invention aims to solve the problem that the propylene oxide in environmental samples such as water, soil and the like in sudden pollution accidents cannot be rapidly, qualitatively and quantitatively detected and analyzed, and provides an analysis method of the propylene oxide in the sudden pollution accidents.
In order to achieve the purpose, the invention is realized by the following technical scheme:
an analysis method of propylene oxide in sudden pollution accidents adopts a technology of combining static headspace and vehicle-mounted gas chromatography/mass spectrometry to carry out on-site rapid and accurate quantitative detection and analysis on propylene oxide in sudden water pollution accidents, takes the static headspace as a pretreatment means, takes experimental water as a solvent, carries out quantitative analysis by an internal standard method, and separates the propylene oxide from internal standard fluorobenzene on a DB-624(20m multiplied by 0.18 mm multiplied by 1 mu m) LTM medium polarity chromatographic column;
the detection conditions are as follows: gas phase parameters: sample inlet temperature: 150 ℃; column flow rate: 1.0ml/min, constant current mode; split-flow sample injection with a split-flow ratio of 20: 1; temperature programming: keeping at 60 deg.C for 10 min;
mass spectrum parameters: MSD transmission line temperature: 250 ℃; ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI voltage: 70eV, scanning mode: selecting an ion scanning SIM;
headspace measurement parameters: heating equilibrium temperature: 60 ℃; temperature of the sample injection needle: 75 ℃; transmission line temperature: 100 ℃; heating balance time: 30 min; headspace bottle pressure 20.7 psi; carrier gas pressure: 24.8 psi.
The method for analyzing the propylene oxide in the sudden pollution accident preferably comprises the following steps:
diluting a propylene oxide standard stock solution to prepare a series of standard solutions of 5.0ug/l, 10.0ug/l, 20.0ug/l, 50.0ug/l, 100ug/l and 200ug/l, taking fluorobenzene as an internal standard, performing static headspace-vehicle-mounted gas chromatography/mass spectrometry, quantifying by using an internal standard method, and making a standard curve by taking a peak area A as a vertical coordinate and a concentration C as a horizontal coordinate;
analyzing and detecting the sample and obtaining a result: dissolving a propylene oxide sample to be detected in water, and measuring the peak area of the propylene oxide sample; and (4) comparing the obtained peak area with the standard curve established in the step (i) to obtain the concentration of the propylene oxide.
Preferably, in the detection, the solubility of propylene oxide in water is increased by salting out to improve the sensitivity of propylene oxide measurement, and the salt added by salting out is anhydrous sodium sulfate.
More preferably, the amount of the anhydrous sodium sulfate added is 3g/10ml of water.
Preferably, an Agilent 5975T LTM-GC/MSD vehicle-mounted gas chromatography/mass spectrometer is selected for testing the vehicle-mounted gas chromatography/mass spectrum. 5975T LTM-GC/MSD vehicle-mounted gas chromatography/mass spectrometer is an instrument for on-site rapid analysis of a low heat capacity LTM chromatographic column module which adopts a heated hyperbolic quadrupole mass filter, a heater and a fused quartz capillary tube of a temperature sensor and a capillary tube protection column, has the characteristics of rapid heating and cooling, good anti-seismic effect, strong mobility, rapid sample analysis and the like, and is suitable for on-site rapid emergency monitoring of sudden pollution accidents.
Compared with the prior art, the invention has the following advantages:
the method for analyzing the propylene oxide in the sudden pollution accident has the characteristics of high temperature rising and falling speed, good anti-seismic effect, strong mobility, high sample analysis speed and the like, and is suitable for field emergency monitoring of the sudden pollution accident.
According to the method for analyzing the propylene oxide in the sudden pollution accident, the DB-624LTM fused quartz capillary chromatographic column is adopted, the propylene oxide and the internal standard fluorobenzene can be effectively separated, the baseline separation between the two components is realized, and the method is effective and reliable; the propylene oxide and the internal standard fluorobenzene can be efficiently separated within 4min, the propylene oxide is quantified by an internal standard method, and the high sensitivity and the high reproducibility are realized;
according to the method for analyzing the propylene oxide in the sudden pollution accident, the interference of inert gases such as argon and carbon dioxide to the propylene oxide is avoided by adopting an MS SIM scanning mode.
Drawings
FIG. 1 is a schematic diagram showing the effect of headspace heating equilibrium temperature on propylene oxide peak area;
FIG. 2 is a schematic graph showing the effect of heating equilibration time on propylene oxide peak area;
FIG. 3 is a graph showing the effect of salts of different ionic strengths on propylene oxide peak area;
FIG. 4 is a graph showing the effect of the amount of sodium sulfate anhydrous added on the propylene oxide peak area;
FIG. 5 is a total ion flow chromatography (TIC) graph of propylene oxide;
FIG. 6 is a graph of a selective ion Scan (SIM) of propylene oxide and fluorobenzene;
reference numerals
1 propylene oxide, 2 fluorobenzene.
Detailed Description
The invention aims to provide an analysis method of propylene oxide in sudden pollution accidents, which is realized by the following technical scheme:
an analysis method of propylene oxide in sudden pollution accidents adopts a technology of combining static headspace and vehicle-mounted gas chromatography/mass spectrometry to carry out on-site rapid and accurate quantitative detection and analysis on propylene oxide in sudden water pollution accidents, takes the static headspace as a pretreatment means, takes experimental water as a solvent, carries out quantitative analysis by an internal standard method, and separates the propylene oxide from internal standard fluorobenzene on a DB-624(20m multiplied by 0.18 mm multiplied by 1 mu m) LTM medium polarity chromatographic column;
the detection conditions are as follows: gas phase parameters: sample inlet temperature: 150 ℃; column flow rate: 1.0ml/min, constant current mode; split-flow sample injection with a split-flow ratio of 20: 1; temperature programming: keeping at 60 deg.C for 10 min;
mass spectrum parameters: MSD transmission line temperature: 250 ℃; ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI voltage: 70eV, scanning mode: selecting an ion scanning SIM;
headspace measurement parameters: heating equilibrium temperature: 60 ℃; temperature of the sample injection needle: 75 ℃; transmission line temperature: 100 ℃; heating balance time: 30 min; headspace bottle pressure 20.7 psi; carrier gas pressure: 24.8 psi.
The propylene oxide and the internal standard fluorobenzene are all completely peaked before 4min, and the temperature programming time is prolonged for qualitatively detecting whether other organic pollutants exist in a pollution accident.
A selective ion Scanning (SIM) mode is adopted to independently scan the quantitative ions 58, the qualitative ions 43 and 57 and the internal standard fluorobenzene qualitative and quantitative ion 96 of the propylene oxide, so that the interference of inert gas argon mass-to-charge ratio (m/z)40 and carbon dioxide m/z44 on the propylene oxide is avoided.
When an internal standard compound is selected, SIM scanning is carried out on epoxypropane, fluorobenzene and 1, 4-dichlorobenzene-d 4 with the same concentration, the peak emergence time of the epoxypropane on a DB-624LTM chromatographic column is 1.842min, the retention time of the fluorobenzene is 3.856min, and the peak emergence time of 1, 4-dichlorobenzene-d 4 is 15.054 min; the diffusion and transmission of pollutants can be controlled more quickly by considering the short monitoring time of monitoring, analyzing and monitoring the epoxy propane in the sudden water pollution accident, and further technical support is provided for an environmental supervision department. Because the peak of the propylene oxide is fast and the propylene oxide and fluorobenzene realize baseline separation, the fluorobenzene is selected as an internal standard in comprehensive consideration.
In selecting the heating equilibrium temperature of the headspace, the influence of the equilibrium temperatures of 45 ℃, 50 ℃, 60 ℃, 70 ℃ and 80 ℃ on the propylene oxide peak area was examined. The influence of the equilibrium temperature is shown in fig. 1, and the results show that the peak area of propylene oxide shows a tendency of increasing and then decreasing with the increase of the equilibrium temperature, and when the equilibrium temperature is 60 ℃, the peak area of propylene oxide reaches the maximum, so that the optimum heating equilibrium temperature of the headspace is selected to be 60 ℃.
The influence of the heating equilibrium time of 15min, 20min, 25min, 30min, 35min and 40min on the peak area of propylene oxide was investigated. As shown in FIG. 2, the length of the heating equilibration time has a significant effect on propylene oxide. The increase rate of the peak area of the propylene oxide is slow after the peak area increases for 30min along with the increase of the heating equilibrium time, and the peak area of the propylene oxide reaches the maximum when the heating equilibrium time is 30 min. During sudden emergency site monitoring, the analysis requirement can be met in a short time. Therefore, the heating balance time is selected to be 30min for other optimization experiments.
The method for analyzing the propylene oxide in the sudden pollution accident preferably comprises the following steps:
diluting a propylene oxide standard stock solution to prepare a series of standard solutions of 5.0ug/l, 10.0ug/l, 20.0ug/l, 50.0ug/l, 100ug/l and 200ug/l, taking fluorobenzene as an internal standard, performing static headspace-vehicle-mounted gas chromatography/mass spectrometry, quantifying by using an internal standard method, and making a standard curve by taking a peak area A as a vertical coordinate and a concentration C as a horizontal coordinate;
fluorobenzene is used as an internal standard compound, and the concentration of the internal standard compound is selected to be the middle concentration of the propylene oxide standard solution, and can be selected to be 50.0 ug/l.
Analyzing and detecting the sample and obtaining a result: dissolving a propylene oxide sample to be detected in water, and measuring the peak area of the propylene oxide sample; and (4) comparing the obtained peak area with the standard curve established in the step (i) to obtain the concentration of the propylene oxide.
Preferably, in the detection, the solubility of propylene oxide in water is increased by salting out to improve the sensitivity of propylene oxide measurement, and the salt added by salting out is anhydrous sodium sulfate.
In selecting the salt to be added by salting out, the influence of salts having different ionic strengths on the propylene oxide peak area was examined. At the same concentration, respectively carrying out anhydrous NaCl, anhydrous KCl and anhydrous Na2SO4Anhydrous K2SO4NaOH and no salt, the results are shown in FIG. 3, when 3g of anhydrous Na is added2SO4The peak area of propylene oxide is maximized. Thus, the optimum salt was determined to be anhydrous Na2SO4。
More preferably, the amount of the anhydrous sodium sulfate added is 3g/10ml of water.
Examine anhydrous Na2SO4The result of the effect of the added amount on the peak area of propylene oxide is shown in fig. 4, the peak area of propylene oxide increases continuously with the increase of the ionic strength of the solution, and the peak area is in a descending trend after the solution is saturated. Anhydrous Na2SO4When the amount of the added water is 3g/10ml, the peak area of propylene oxide reaches the maximum value, so that anhydrous Na is selected2SO4The amount added was 3g/10ml of water.
Preferably, an Agilent 5975T LTM-GC/MSD vehicle-mounted gas chromatography/mass spectrometer is selected for testing the vehicle-mounted gas chromatography/mass spectrum.
The invention is further described with reference to specific examples.
Example 1
An analysis method of propylene oxide in sudden pollution accidents adopts a technology of combining static headspace and vehicle-mounted gas chromatography/mass spectrometry to carry out on-site rapid and accurate quantitative detection and analysis on propylene oxide in sudden water pollution accidents, takes the static headspace as a pretreatment means, takes experimental water as a solvent, carries out quantitative analysis by an internal standard method, and separates the propylene oxide from internal standard fluorobenzene on a DB-624(20m multiplied by 0.18 mm multiplied by 1 mu m) LTM medium polarity chromatographic column;
the detection conditions are as follows: gas phase parameters: sample inlet temperature: 150 ℃; column flow rate: 1.0ml/min, constant current mode; split-flow sample injection with a split-flow ratio of 20: 1; temperature programming: keeping at 60 deg.C for 10 min;
mass spectrum parameters: MSD transmission line temperature: 250 ℃; ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI voltage: 70eV, scanning mode: selecting an ion scanning SIM;
headspace measurement parameters: heating equilibrium temperature: 60 ℃; temperature of the sample injection needle: 75 ℃; transmission line temperature: 100 ℃; heating balance time: 30 min; headspace bottle pressure 20.7 psi; carrier gas pressure: 24.8 psi.
And diluting the standard stock solution of the propylene oxide step by step to prepare a standard solution of 10.0 ug/ml. Static headspace-vehicle LTM-GC/MSD analysis was performed under the above conditions, the total ion current chromatogram is shown in fig. 5, the selective ion scan is shown in fig. 6, and the horizontal axis is time/min and the vertical axis is abundance in fig. 5 and 6.
The results of fig. 5 and 6 show that both propylene oxide and fluorobenzene can achieve good baseline separation within 4min, and meanwhile, due to the adoption of a selective ion scanning mode and an internal standard method for quantification, the influence of inert gases such as argon and carbon dioxide, fine changes of mass spectrometer ionization efficiency and the like on the chromatographic peak of propylene oxide and the sensitivity of measurement are avoided.
In the experiment, the propylene oxide qualitative and quantitative ions, a mass spectrometer scanning mode, the headspace heating temperature, the balance time, the salt types and the addition amount are optimally selected, the propylene oxide is measured by an internal standard method by using a selective ion Scanning (SIM) mode, and the quantitative ions 58, the qualitative ions 43 and 57 and the internal standard fluorobenzene qualitative and quantitative ions 96 of the propylene oxide are separately scanned, so that the interference of inert gases argon mass-to-charge (m/z)40 and carbon dioxide m/z44 on the propylene oxide can be effectively avoided. Thereby greatly improving the sensitivity of the propylene oxide determination.
Example 2
An analysis method of propylene oxide in sudden pollution accidents adopts a technology of combining static headspace and vehicle-mounted gas chromatography/mass spectrometry to carry out on-site rapid and accurate quantitative detection and analysis on propylene oxide in sudden water pollution accidents, takes the static headspace as a pretreatment means, takes experimental water as a solvent, carries out quantitative analysis by an internal standard method, and separates the propylene oxide from internal standard fluorobenzene on a DB-624(20m multiplied by 0.18 mm multiplied by 1 mu m) LTM medium polarity chromatographic column; the method specifically comprises the following steps:
diluting a propylene oxide standard stock solution to prepare a series of standard solutions of 5.0ug/l, 10.0ug/l, 20.0ug/l, 50.0ug/l, 100ug/l and 200ug/l, taking fluorobenzene as an internal standard, performing static headspace-vehicle-mounted gas chromatography/mass spectrometry, quantifying by using an internal standard method, and making a standard curve by taking a peak area A as a vertical coordinate and a concentration C as a horizontal coordinate; fluorobenzene is used as an internal standard compound, and the concentration of the internal standard compound is selected to be the middle concentration of the propylene oxide standard solution, and can be selected to be 50.0 ug/l.
The detection conditions during the test were: gas phase parameters: sample inlet temperature: 150 ℃; column flow rate: 1.0ml/min, constant current mode; split-flow sample injection with a split-flow ratio of 20: 1; temperature programming: keeping at 60 deg.C for 10 min;
mass spectrum parameters: MSD transmission line temperature: 250 ℃; ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI voltage: 70eV, scanning mode: selecting an ion scanning SIM;
headspace measurement parameters: heating equilibrium temperature: 60 ℃; temperature of the sample injection needle: 75 ℃; transmission line temperature: 100 ℃; heating balance time: 30 min; headspace bottle pressure 20.7 psi; carrier gas pressure: 24.8 psi.
Researches show that the concentration and the ordinate of the propylene oxide present a good linear relationship, and linear regression is carried out to obtain a regression equation. And (3) calculating the detection limit, linear equation, correlation coefficient and detection limit of the standard substance by using MDL ═ t (n-1,0.99) S. Calibration curve for propylene oxide: y 5.388 x 10-2x + 0.1255; the correlation coefficient r is 0.9999, and the detection limit of the method is 1.5 ug/l. Therefore, the propylene oxide has good linear relation with the peak area within the range of 5.00ug/l to 200 ug/l; the method has a lower detection limit, and can effectively detect the propylene oxide in sudden pollution accidents.
Analyzing and detecting the sample and obtaining a result: dissolving a propylene oxide sample to be detected in water, and measuring the peak area of the propylene oxide sample; and (4) comparing the obtained peak area with the standard curve established in the step (i) to obtain the concentration of the propylene oxide.
1. And (3) inspecting the precision of the chromatographic system, continuously feeding a standard solution with the concentration of 20.0ug/l of propylene oxide under the linear relation test item into six needles, and inspecting the precision of the method, wherein the precision results of 6 times of measurement are respectively 22.2ug/l, 22.9ug/l, 22.2ug/l, 21.1ug/l, 20.9ug/l and 21.4ug/l, the RSD of the propylene oxide is 3.55 percent, and the method has good precision.
From the above data, it can be seen that the RSD of propylene oxide is much less than 10%, and the method is of good precision.
2. Intermediate precision investigation of the above chromatographic system:
the results of the above experiments were repeated by different persons under different chromatographic principle instruments with intermediate precision using measured concentrations are as follows. The results of the intermediate precision test of the propylene oxide on the first instrument are respectively 22.2ug/l, 22.9ug/l, 22.2ug/l, 21.1ug/l, 20.9ug/l and 21.4ug/l, and the RSD of the propylene oxide is 3.55%; the results of intermediate precision tests on the second instrument are 23.3ug/l, 21.9ug/l, 22.1ug/l, 23.6ug/l, 22.4ug/l and 21.4ug/l respectively, and the RSD of the propylene oxide is 3.77%;
from the above data, it can be seen that the RSD of propylene oxide is much less than 10%, and the method has good intermediate precision.
3. Accuracy survey of the above chromatographic system
Taking the propylene oxide under the linear relation test item, respectively adding 10.0ug/l, 50.0ug/l and 150ug/l into blank samples, carrying out headspace heating balance pretreatment, carrying out quantitative analysis by adopting an internal standard method, and respectively calculating the recovery rate of each component. The results are shown in Table 1.
TABLE 1 propylene oxide recovery test results
As can be seen from the table above, the average recovery rates of nine samples under three concentrations are 96.5% -103.5%, and the RSD of the recovery rates of 9 samples are within 10%, so that the quality control requirement is met, and the accuracy of the chromatographic method meets the requirement.
In conclusion, the method can effectively measure the propylene oxide, can accurately and quickly measure the propylene oxide on site, is simple, quick, accurate and effective, has high precision, and can measure the content of the propylene oxide in sudden emergency accidents.
Claims (5)
1. A method for analyzing propylene oxide in sudden pollution accidents is characterized by comprising the following steps: the method comprises the steps of performing on-site rapid and accurate quantitative detection and analysis on propylene oxide in sudden water pollution accidents by adopting a static headspace and vehicle-mounted gas chromatography/mass spectrometry combined technology, performing quantitative analysis by an internal standard method by taking the static headspace as a pretreatment means and experimental water as a solvent, and separating the propylene oxide from internal standard fluorobenzene on a DB-624LTM medium-polarity chromatographic column;
the detection conditions are as follows: gas phase parameters: sample inlet temperature: 150 ℃; column flow rate: 1.0ml/min, constant current mode; split-flow sample injection with a split-flow ratio of 20: 1; temperature programming: keeping at 60 deg.C for 10 min;
mass spectrum parameters: MSD transmission line temperature: 250 ℃; ion source temperature: 230 ℃, quadrupole temperature: 150 ℃; EI voltage: 70eV, scanning mode: selecting an ion scanning SIM;
headspace measurement parameters: heating equilibrium temperature: 60 ℃; temperature of the sample injection needle: 75 ℃; transmission line temperature: 100 ℃; heating balance time: 30 min; headspace bottle pressure 20.7 psi; carrier gas pressure: 24.8 psi.
2. The method for analyzing propylene oxide in sudden pollution accident according to claim 1, wherein: the method comprises the following steps:
3. The method for analyzing propylene oxide in sudden pollution accident according to claim 1, wherein: during detection, the solubility of the propylene oxide in water is increased by salting out, the measurement sensitivity of the propylene oxide is improved, and the salt added by salting out is anhydrous sodium sulfate.
4. The method for analyzing propylene oxide in sudden pollution accident according to claim 3, wherein: the amount of anhydrous sodium sulfate added was 3g/10ml of water.
5. The method for analyzing propylene oxide in sudden pollution accident according to claim 1, wherein: an Agilent 5975T LTM-GC/MSD vehicle-mounted gas chromatography/mass spectrometer is selected for testing the vehicle-mounted gas chromatography/mass spectrum.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728164A (en) * | 2012-10-16 | 2014-04-16 | 辽宁奥克化学股份有限公司 | Method for preparing epoxy compound standard solution and method for measuring concentration of epoxy compound |
| CN105372365A (en) * | 2015-10-30 | 2016-03-02 | 中国烟草总公司郑州烟草研究院 | Method for online detection of ethylene oxide and propylene oxide in smoke of cigarettes |
| CN110220998A (en) * | 2019-07-30 | 2019-09-10 | 南京卡文迪许生物工程技术有限公司 | The detection method of residual epoxy propane in a kind of drug |
| CN110221004A (en) * | 2019-07-18 | 2019-09-10 | 青岛琛蓝海洋生物工程有限公司 | A kind of detection method and application of epoxychloropropane |
-
2021
- 2021-12-27 CN CN202111608654.9A patent/CN114324684A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728164A (en) * | 2012-10-16 | 2014-04-16 | 辽宁奥克化学股份有限公司 | Method for preparing epoxy compound standard solution and method for measuring concentration of epoxy compound |
| CN105372365A (en) * | 2015-10-30 | 2016-03-02 | 中国烟草总公司郑州烟草研究院 | Method for online detection of ethylene oxide and propylene oxide in smoke of cigarettes |
| CN110221004A (en) * | 2019-07-18 | 2019-09-10 | 青岛琛蓝海洋生物工程有限公司 | A kind of detection method and application of epoxychloropropane |
| CN110220998A (en) * | 2019-07-30 | 2019-09-10 | 南京卡文迪许生物工程技术有限公司 | The detection method of residual epoxy propane in a kind of drug |
Non-Patent Citations (7)
| Title |
|---|
| 张敬轩;李挥;蔡立鹏;范斌;张岩;: "顶空进样-气相色谱-质谱法检测清洁类化妆品中环氧乙烷和环氧丙烷残留量", 分析化学, no. 08, pages 2 - 2 * |
| 段梦茹;何东升;孙会敏;熊晔蓉;涂家生;: "气相色谱法检测泊洛沙姆188中环氧化物杂质", 药学研究, no. 06 * |
| 王安祥;徐广洲;王坤;王春蕾;: "吹扫捕集-气相色谱-质谱法同时测定水中11种醚类化合物", 理化检验(化学分册), no. 07, pages 1 - 1 * |
| 王海波;王倩;王雪芹;李杨;: "GC-MS法测定奥硝唑注射液中环氧丙烷的含量", 广东药科大学学报, no. 01 * |
| 王琪慧;李铭;詹雪芳;: "顶空气相色谱-质谱联用法测定清洁类化妆品中的环氧丙烷", 日用化学工业, no. 01 * |
| 肖洋;王新娟;韩伟;郝亮;张媛;: "顶空进样-便携式气相色谱-质谱法快速测定水中挥发性有机物", 理化检验(化学分册), no. 07 * |
| 薛建平;: "顶空-气质联用法同时测定纺织品中环氧乙烷、环氧丙烷和二氧六环", 上海纺织科技, no. 11 * |
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