CN101162217A - Gas-chromatography double investigation apparatus method and system for determining chloroform, carrene, ethinyltrichloride 1, 4-dioxane residual quantity - Google Patents
Gas-chromatography double investigation apparatus method and system for determining chloroform, carrene, ethinyltrichloride 1, 4-dioxane residual quantity Download PDFInfo
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- CN101162217A CN101162217A CNA200610117139XA CN200610117139A CN101162217A CN 101162217 A CN101162217 A CN 101162217A CN A200610117139X A CNA200610117139X A CN A200610117139XA CN 200610117139 A CN200610117139 A CN 200610117139A CN 101162217 A CN101162217 A CN 101162217A
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Abstract
The invention relates to a measuring method and system of a gas chromatographic double detector for chloroform, methylene dichloride, chlorylene and 1, 4-dioxanes. The measuring method is that: one end of a tee current divider is connected with an outlet of a capillary gas chromatographic column, gas component from the chromatographic column flows separately to a hydrogen flame ionization detector and a microcell electron capture detector. The hydrogen flame ionization detector detects the response chromatogram maps of the four menstruums; the microcell electron capture detector detects the response chromatogram maps of other menstruums except the 1, 4-dioxanes. The measuring system comprises a gas chromatograph, the hydrogen flame ionization detector, the microcell electron capture detector and the tee current divider. With the invention, on the premise that the measuring sensitivity of the methylene dichloride and the 1, 4-dioxanes is basically kept, the measuring sensitivity of the chloroform and the chlorylene is greatly improved in single measurement, thereby guaranteeing the reliability and accuracy of the measuring result of the organic menstruum residual quantity of products.
Description
Technical field
The present invention relates to analytical test chloroform, methylene chloride, triclene and 1, the method of 4-dioxane, specifically be meant and adopt gas chromatography dual-detector method to carry out chloroform, methylene chloride, triclene and 1 in the product (comprising medicine and cosmetics), the method for measuring and the system of four kinds of organic solvent minimal residues of 4-dioxane.
Background technology
Chloroform, methylene chloride, triclene and 1 in the product (medicine or cosmetics), the residual quantity detection method of 4-dioxane adopts gas chromatography-flame ionization ditector to carry out usually, for example according to American Pharmacopeia＜467〉method V, wherein the response of chloroform and triclene influences the result and judges near detectability; According to American Pharmacopeia＜467〉method IV detect, though wherein the response of chloroform and triclene slightly improves, this method still can not fine satisfied detection requirement.In order effectively to control the residual quantity of above-mentioned four kinds of solvents in the product (comprising medicine and cosmetics), need on existing technical standard basis, set up sensitivity and detection means more accurately.
Summary of the invention
The object of the present invention is to provide a kind of employing gas chromatography dual-detector method, to chloroform, methylene chloride, triclene and 1 in the product, the residual quantity of 4-dioxane detects.
The present invention exports the distributing T-pipe device, flame ionization ditector, four kinds of organic solvents of little pond electron capture detector separation determination by gas chromatograph.
The gas chromatography dual-detector assay method of above-mentioned four kinds of organic solvent residuals, it is characterized in that distributing T-pipe device one end is linked to each other with gas phase capillary chromatographic column exit, make gas composition shunting, flow to flame ionization ditector and little pond electron capture detector respectively from chromatographic column.Flame ionization ditector detects the chromatogram of above-mentioned four kinds of solvent responses; Little pond electron capture detector detects to remove and does not contain 1, the chromatogram of other solvent responses of 4-dioxane.
The distributing T-pipe device of assay method of the present invention is adjustable shunt preferably, is made up of Control Component, triplate line, the bubble-tight graphite gasket of assurance device and connecting pipe.When tommy screwed on the shunt, shunt one brought out mouth and will be plugged, and becomes the bipass road; After the shunt tommy was outwarded winding, shunt had two exit passageways, triplate line, and the ratio of the component on two exit passageways can be regulated by tommy.
The distributing T-pipe device of assay method of the present invention can integral body directly be put into gas chromatograph stove case, or it is installed on the tank wall, and the threeway part is in the stove case, and Control Component is exposed to outside the stove case.
The component distribution pipeline of assay method of the present invention is realized by the distributing T-pipe device.The chromatographic column endpiece links to each other with distributing T-pipe device inlet end all the time, and two endpiece of distributing T-pipe device link to each other with flame ionization ditector interface end, little pond electron capture detector interface end respectively with two connecting pipes.
The connecting pipe of assay method of the present invention is preferably the deactivation elastic quartz capillary tube.
The gas chromatograph of assay method of the present invention is for being equipped with flame ionization ditector (FID) and little pond electron capture detector (μ-ECD), and the distributing T-pipe device is formed.
Chloroform of the present invention, methylene chloride, triclene and 1, the gas chromatography dual-detector of 4-dioxane is measured system, comprises; Gas chromatograph, measure described four kinds of solvent responses the chromatogram flame ionization ditector, detect and remove 1, chromatogram little pond electron capture detector of other solvent responses that the 4-dioxane is outer and the distributing T-pipe device that carries out the component shunting.
Above-mentioned detection system, being preferably described distributing T-pipe device is adjustable distributing T-pipe device, this is adjustable, and the distributing T-pipe device comprises, Control Component, triplate line, the bubble-tight graphite gasket of assurance device and as the deactivation elastic quartz capillary tube of connecting pipe.This scalable distributing T-pipe device can integral body directly be put into gas chromatograph stove case, or it is installed on the tank wall, and the threeway part is in the stove case, and Control Component is exposed to outside the stove case.The described adjustable distributing T-pipe device of said detecting system can be realized the bipass road and the triplate line of distributing T-pipe device, promptly has two switchings between the exit passageway, and can adjust the ratio of two components on the exit passageway.
Gas chromatograph of the present invention preferably is equipped with the corresponding work station software, can obtain two detection collection of illustrative plates on the detecting device simultaneously.
Method and system of the present invention, preferred pin is to medicine and cosmetics and make chloroform, methylene chloride, triclene and 1 in their raw material, four kinds of residual organic solvent limit tests of 4-dioxane and assay.
The invention has the advantages that by the dual-detector method not to influence methylene chloride and 1, under the prerequisite of the detection sensitivity of 4-dioxane, improves the detection sensitivity of other two kinds of solvents (chloroform and triclene) greatly.Overcome existing detection method defective, and to need to have avoided the loaded down with trivial details process of at least twice difference sample detection, guaranteed result's accuracy and reliability.In addition, the chromatogram that the present invention obtains and result's report also are different from the gas chromatography diagram form of common gained with the combination collection of illustrative plates that comprises that simultaneously flame ionization ditector and little pond electron capture detector obtain.
Description of drawings
Fig. 1 is for relating to three vent passage connection sketch among the present invention.Wherein 1 is tommy, and 2 are and the terminal import that links to each other of chromatographic column, and 3 is the outlet that links to each other with the connecting pipe that leads to flame ionization ditector, and 4 is the outlet that links to each other with the connecting pipe that leads to little pond electron capture detector.
Fig. 2 relates to gas flow pipeline structure synoptic diagram among the present invention.Gas composition is after the terminal outflow of chromatographic column, adjusting by the distributing T-pipe device, flow to two detecting devices respectively, 1 is injection port, and 2 is capillary chromatographic column, and 3 is the distributing T-pipe device, 4,5 is connecting pipe, 6 is flame ionization ditector, and 7 is little pond electron capture detector, and 8 is gas chromatograph stove case.
The collection of illustrative plates combination collection of illustrative plates that the dual-detector that Fig. 3 obtains for the present invention obtains, and the comparison collection of illustrative plates of measuring with single detecting device.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, and see also all accompanying drawings.
Connection to three vent passage described in the inventive method is described.Fig. 1 is three a vent passage connection sketch.
Quartz capillary chromatographic column is passed the nut that has graphite gasket, insert the import 2 of distributing T-pipe device, tightening nuts; One end that will lead to the connecting pipe of flame ionization ditector passes the nut that has graphite gasket, inserts the outlet 3 of distributing T-pipe device; One end that will lead to the connecting pipe of little pond electron capture detector passes the nut that has graphite gasket, inserts the outlet 4 of distributing T-pipe device; At last the other end of two connecting pipes is linked to each other with the inlet of two detecting devices respectively, finish the shunting transformation of gas circuit.
The dual-detector of gas chromatograph described in the inventive method detection method is described.Fig. 2 is a gas chromatograph dual-detector detection method device sketch.
Experiment adopts the gas chromatograph that flame ionization ditector and little pond electron capture detector are installed to analyze, having selected specification is 30 meters * 0.53 millimeter * DB-624 fused-silica capillary column of 3.0 microns (thickness), column temperature operating conditions: 40 ℃ (keeping 23 minutes), be warming up to 80 ℃ (keeping 10 minutes) with 50 ℃ of/minute clock rate.Other operating conditionss are: 140 ℃ of injector temperatures, column cap are pressed 0.02 MPa (MPa), split ratio: 5: 1; Flame ionization ditector (FID) temperature: 260 ℃, FID hydrogen flowing quantity: 30 ml/min, FID air mass flow: 350 ml/min, FID make-up gas? (N
2) flow: 20 ml/min; Little pond electron capture detector (temperature of μ-ECD): 250 ℃, μ-ECD make-up gas? (N
2) flow: 60 ml/min; Sample size: 1000 microlitres, use automatic headspace sampling instrument sample introduction.Two connecting pipe internal diameters of distributing T-pipe device are 0.22 micron.
After the distributing T-pipe device installs, tommy is screwed out 4mm length by tight condition.Start gas chromatograph and headspace sampling instrument, auto injection, carrier gas is carried component to be checked and is entered chromatographic column, after post separates, enter the shunt pipeline, gas composition divides two-way to enter FID and μ-ECD detecting device respectively, the detector recording signal, and in chromatographic work station, form collection of illustrative plates.
Performance to the coupling of the dual-detector of gas chromatograph described in the inventive method is described.Fig. 3 measures the comparison collection of illustrative plates of measuring with conventional single detecting device for the dual-detector coupling.
By pharmacopeia prescribed limit standard, preparation limit contrast solution wherein contains methylene chloride 12 mcg/ml, chloroform 1.2 mcg/ml, triclene 1.6 mcg/ml, 1,4-dioxane 7.6 mcg/ml are pressed example 2 described condition analysiss, obtain a chromatogram 1.Chromatogram 1 top is μ-ECD detection figure, and the below is FID detection figure.A is the methylene chloride peak, and B is the chloroform peak, and C is the triclene peak, and D is 1,4-dioxane peak.
Press American Pharmacopeia＜467〉method IV, identical limit contrast solution obtains a chromatogram by example 2 described condition analysiss
Fig. 2, A are the methylene chloride peak, and B is the chloroform peak, and C is the triclene peak, and D is 1,4-dioxane peak.
If estimate detection sensitivity with the signal to noise ratio (S/N ratio) parameter of each solvent, with American Pharmacopeia＜467〉method IV contrasts, guaranteeing 1, under the prerequisite of the necessary detection sensitivity of 4-dioxane, the sensitivity of chloroform on μ-ECD has improved more than 100 times in the inventive method, and the sensitivity of triclene on μ-ECD has improved more than 50 times.
Claims (7)
1. a chloroform, methylene chloride, triclene and 1, the gas chromatography dual-detector assay method of 4-dioxane is characterized in that, comprising:
Make gas composition shunting, flow to flame ionization ditector and little pond electron capture detector respectively from chromatographic column;
Flame ionization ditector detects the chromatogram of above-mentioned four kinds of solvent responses, and little pond electron capture detector detects and removes 1, the chromatogram of other solvent responses that the 4-dioxane is outer.
2. the method for claim 1, it is characterized in that the shunting of described component is to realize by adjustable distributing T-pipe device, this is adjustable distributing T-pipe device, comprise Control Component, triplate line, the bubble-tight graphite gasket of assurance device and as the deactivation elastic quartz capillary tube of connecting pipe.
3. method as claimed in claim 2 is characterized in that, realizes the bipass road of distributing T-pipe device and the switching between the triplate line by described Control Component, and can adjust the ratio of two components on the exit passageway.
4. a chloroform, methylene chloride, triclene and 1, the gas chromatography dual-detector detection system of 4-dioxane, it is characterized by, comprise: gas chromatograph, the chromatogram flame ionization ditector that detects described four kinds of solvent responses, detection remove 1, chromatogram little pond electron capture detector of other solvent responses that the 4-dioxane is outer and the distributing T-pipe device that carries out the component shunting.
5. detection system as claimed in claim 4, it is characterized in that, described distributing T-pipe device is adjustable distributing T-pipe device, and this is adjustable, and the distributing T-pipe device comprises, Control Component, triplate line, the bubble-tight graphite gasket of assurance device and as the deactivation elastic quartz capillary tube of connecting pipe.
6. detection system as claimed in claim 5 is characterized in that, described adjustable distributing T-pipe device can be realized the bipass road of distributing T-pipe device and the switching between the triplate line, and can adjust the ratio of two components on the exit passageway.
7. detection system as claimed in claim 4 is characterized in that, described gas chromatograph can obtain described flame ionization ditector simultaneously and two of little pond electron capture detectors detect collection of illustrative plates.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200610117139XA CN101162217A (en) | 2006-10-13 | 2006-10-13 | Gas-chromatography double investigation apparatus method and system for determining chloroform, carrene, ethinyltrichloride 1, 4-dioxane residual quantity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200610117139XA CN101162217A (en) | 2006-10-13 | 2006-10-13 | Gas-chromatography double investigation apparatus method and system for determining chloroform, carrene, ethinyltrichloride 1, 4-dioxane residual quantity |
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| CN101162217A true CN101162217A (en) | 2008-04-16 |
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| CNA200610117139XA Pending CN101162217A (en) | 2006-10-13 | 2006-10-13 | Gas-chromatography double investigation apparatus method and system for determining chloroform, carrene, ethinyltrichloride 1, 4-dioxane residual quantity |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102043027A (en) * | 2010-10-26 | 2011-05-04 | 上海烟草（集团）公司 | Method for evaluating absorbing performance of cigarette filter absorbing agent and testing system thereof |
| CN104458986A (en) * | 2014-10-29 | 2015-03-25 | 中国科学院广州地球化学研究所 | Gas chromatography multichannel sample introduction system and realized atmosphere detection method thereof |
| CN104569246A (en) * | 2014-12-08 | 2015-04-29 | 江苏泰洁检测技术有限公司 | Detection method for measuring halogenated hydrocarbon compounds by gas chromatographic method |
| CN112014487A (en) * | 2019-05-30 | 2020-12-01 | 特丰制药有限公司 | Method for determining chloral hydrate or chloralkane content in preparation thereof |
-
2006
- 2006-10-13 CN CNA200610117139XA patent/CN101162217A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102043027A (en) * | 2010-10-26 | 2011-05-04 | 上海烟草（集团）公司 | Method for evaluating absorbing performance of cigarette filter absorbing agent and testing system thereof |
| CN102043027B (en) * | 2010-10-26 | 2013-04-10 | 上海烟草集团有限责任公司 | Method for evaluating absorbing performance of cigarette filter absorbing agent and testing system thereof |
| CN104458986A (en) * | 2014-10-29 | 2015-03-25 | 中国科学院广州地球化学研究所 | Gas chromatography multichannel sample introduction system and realized atmosphere detection method thereof |
| CN104569246A (en) * | 2014-12-08 | 2015-04-29 | 江苏泰洁检测技术有限公司 | Detection method for measuring halogenated hydrocarbon compounds by gas chromatographic method |
| CN112014487A (en) * | 2019-05-30 | 2020-12-01 | 特丰制药有限公司 | Method for determining chloral hydrate or chloralkane content in preparation thereof |
| WO2020239054A1 (en) * | 2019-05-30 | 2020-12-03 | 特丰制药有限公司 | Method for determining chloralkane content in chloral hydrate or preparation thereof |
| CN112014487B (en) * | 2019-05-30 | 2022-02-22 | 特丰制药有限公司 | Method for determining chloral hydrate or chloralkane content in preparation thereof |
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Open date: 20080416 |