CN106404934A - Method for detecting phthalic acid di-n-propyl ester in washing product - Google Patents
Method for detecting phthalic acid di-n-propyl ester in washing product Download PDFInfo
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- CN106404934A CN106404934A CN201610726042.2A CN201610726042A CN106404934A CN 106404934 A CN106404934 A CN 106404934A CN 201610726042 A CN201610726042 A CN 201610726042A CN 106404934 A CN106404934 A CN 106404934A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention relates to a method for detecting phthalic acid di-n-propyl ester in a washing product, and the method is particularly as follows: a sample to be detected is prepared, and a gas chromatography-mass spectrometry method is used to detect; gas chromatographic conditions are as follows: sample inlet temperature is 280-320 DEG C, chromatographic column flow rate is 0.5-3mL / min; sample feeding amount is 0.5-3 mu L, chromatographic column initial column temperature is 100-130 DEG C, chromatographic column temperature is held for 1-3min and then gradiently risen to 280-300 DEG C; mass spectrometry conditions are as follows: an ion source is bombarded by electrons, trap temperature is 200-250 DEG C; chromatography-mass spectrometry interface temperature is 260-300 DEG C, an ion scanning monitoring mode is selected, and quantitative ion is m/z100-m/z150. The method combines the advantages of the gas chromatography and the mass spectrometry, separation, identification and quantification of the sample can be completed simultaneously, and the method has the advantages of high resolution, high sensitivity, strong discrimination ability and good repeatability and accuracy.
Description
Technical field
The present invention relates to a kind of detection method of n-propyl phthalate, adjacent benzene in more particularly, to a kind of articles for washing
The detection method of dioctyl phthalate di-n-propyl ester, belongs to chemical analysis technical field.
Background technology
N-propyl phthalate is one of phthalic acid ester, is a kind of important raw material of industry, and application is wide
General.But, its toxicity is larger, has teratogenesis and embryotoxicity, and impact is internal to secrete, and leads to cancer cell multiplication etc..With
When, it plays the effect of similar female hormone in human body, the semen volume of man and sperm quantity can be made to reduce, meeting when serious
Lead to carcinoma of testis；It can also affect on the reproductive system of women, increases the probability that women suffers from breast cancer.However, in the last few years, adjacent
Phthalic acid di-n-propyl ester is abused by industry-by-industry, the n-propyl phthalate detection especially in articles for washing class
Rate severe overweight.And articles for washing, as a kind of consumer goods of people's daily life, has huge consumption market.Therefore, adjacent
The safety problem of phthalic acid di-n-propyl ester gradually attracts attention.
In view of articles for washing using increasingly extensive, the water of n-propyl phthalate in the contact articles for washing of people
Put down and be also gradually increased.Accordingly, it would be desirable to strengthen the actual dose of n-propyl phthalate in articles for washing is analyzed and
Control, preferably to protect the health of consumer.
Content of the invention
The purpose of the present invention is for the above-mentioned problems in the prior art it is proposed that a kind of detection speed is fast, sample
The detection method of n-propyl phthalate in the articles for washing that pretreatment process is simple, the range of linearity is wide.
The purpose of the present invention can be realized by following technical proposal：N-propyl phthalate in a kind of articles for washing
Detection method, described detection method is：Prepare test specimens to be checked, detected using gas chromatography-mass spectrography；
Wherein, GC conditions are：Injector temperature is 280-320 DEG C, and chromatogram column flow is 0.5-3mL/min, sample
Product sample size is 0.5-3 μ L, and chromatographic column initial column temperature is 100-130 DEG C, and after keeping 1-3min, gradient rises to 280-300 DEG C；
Mass Spectrometry Conditions are：Using electron impact ion source, trap temperature is 200-250 DEG C；
Chromatography-mass spectroscopy interface temperature is 260-300 DEG C, selects ion scan monitoring pattern, and quota ion is m/z 100-
m/z 180.
The present invention is detected to the n-propyl phthalate in articles for washing using gas chromatography-mass spectrography, will
Gas chromatograph is connected by interface module with mass spectrograph, the means being separated as sample using gas-chromatography, preparing, and mass spectrum is made
On-line checking means for gas-chromatography carry out qualitative and quantitative analysis, combine gas-chromatography and mass spectrographic advantage, can be simultaneously complete
Become separation, identification and the quantitation of sample, there is high-resolution, high sensitivity and strong distinguishing ability.
In the detection method of n-propyl phthalate in a kind of above-mentioned articles for washing, the fixing phase of gas-chromatography
For methyl-polysiloxane, the wherein content of phenyl is 2%-10%.The content of phenyl is higher, and the nonpolar of fixing phase is got over
By force；Conversely, then fixing phase is nonpolar weaker.Suitable phenyl content is conducive to the separation of target compound.So, this
The phenyl content of bright fixing phase needs to control within the above range.
In the detection method of n-propyl phthalate in a kind of above-mentioned articles for washing, the column length of chromatographic column is
30m, column internal diameter is 0.25mm.Increase column length favourable to improving separating degree, but the retention time of component extends, and column resistance increases
Plus, it is awkward.So, column length is defined to 30m by the present invention, can meet detached purpose, when being conducive to shortening analysis again
Between.
In the detection method of n-propyl phthalate in a kind of above-mentioned articles for washing, the gradient increased temperature of chromatographic column
Process is：First it is warming up to 180-220 DEG C with 8-15 DEG C/min, then be warming up to 250-260 DEG C with 3-8 DEG C/min, finally again with 8-
15 DEG C/min is warming up to 280-300 DEG C, keeps 5-10min.Because, too fast heating rate be unfavorable for object and impurity point
From, and heating rate too slow then analysis time is long.The heating rate of chromatographic column of the present invention is relatively reasonable, both can guarantee that object
Separate with impurity, analysis time will not be made again long.
In the detection method of n-propyl phthalate in a kind of above-mentioned articles for washing, the carrier gas kind of gas-chromatography
Class is helium, and carrier gas flux is 0.5-3mL/min.The control of the selection of type carrier gases and flow velocity has a certain impact to post effect.
Molar quality can suppress greatly the longitudinal diffusion of sample, improves post effect.When flow rate of carrier gas is larger, resistance to mass tranfer item rises mainly
Effect, the present invention, using the carrier gas helium of less molal weight, can reduce resistance to mass tranfer, improves post effect.
In the detection method of n-propyl phthalate in a kind of above-mentioned articles for washing, the gasification temperature of gas-chromatography
Spend for 250 DEG C.The control of gasification temperature should ensure that sample can be gasified totally, and can not make sample because of gasification temperature is too high again
Decompose.
In the detection method of n-propyl phthalate in a kind of above-mentioned articles for washing, described trap temperature is 230
℃.The present invention further preferred trap temperature is 230 DEG C, because too high or too low ion trap temperature is all unfavorable for target chemical combination
The ionization of thing.
In the detection method of n-propyl phthalate in a kind of above-mentioned articles for washing, described chromatography-mass spectroscopy connects
Mouth temperature is 280 DEG C.The further preferred chromatography-mass spectroscopy interface temperature of the present invention can guarantee that sample does not condense in this region.
Compared with prior art, the present invention to the phthalic acid two in articles for washing is just using gas chromatography-mass spectrography
Propyl ester is detected, gas chromatograph is connected by interface module with mass spectrograph, is separated as sample using gas-chromatography, prepares
Means, mass spectrum is carried out qualitative and quantitative analysis as the on-line checking means of gas-chromatography, combines gas-chromatography and mass spectrum
Advantage, separation, identification and the quantitation of sample can be completed simultaneously, there is high-resolution, high sensitivity and strong distinguishing ability, repeat
Property and accuracy are preferable.
Brief description
Fig. 1 is the selection ion scan chromatogram of n-propyl phthalate standard liquid of the present invention.
Specific embodiment
The following is the specific embodiment of the present invention, and be described with reference to the drawings technical scheme is further retouched
State, but the present invention is not limited to these embodiments.
Embodiment 1：
Standard liquid is prepared：1g/L.
Weigh n-propyl phthalate standard items 10mg, after the dissolving of a small amount of ethyl acetate, use ethyl acetate constant volume
To 10mL volumetric flask, it is configured to the standard liquid of 1mg/mL, keep in Dark Place in 4 DEG C.Ethyl acetate stepwise dilution is used during use
Standard working solution needed for one-tenth.
Sample is prepared and is detected：
Weigh 0.5g liquid detergent to be placed in 10mL colorimetric cylinder, be settled to 10mL with ethyl acetate, mix and carry after ultrasonic wave
Take extraction 5min in device, after extract is filtered with 0.45 μm of filter, take 1mL filtrate as analysis sample, in gas chromatography-mass spectrum
It is measured under combined instrument condition of work.
Testing conditions：
GC conditions are：The column length of chromatographic column is 30m, and column internal diameter is 0.25mm, and chromatogram column flow is 1mL/min.
The fixing phase of gas-chromatography is methyl-polysiloxane, and wherein the content of phenyl is 5%.The type carrier gases of gas-chromatography are helium
Gas, carrier gas flux is 1mL/min.The gasification temperature of gas-chromatography is 250 DEG C.Injector temperature is 300 DEG C, and sample injection volume is
1 μ L, does not shunt.Chromatographic column initial column temperature is 120 DEG C, is first warming up to 200 DEG C with 10 DEG C/min after keeping 2min, then with 5 DEG C/
Min is warming up to 260 DEG C, is finally warming up to 280 DEG C with 10 DEG C/min again, keeps 6min.
Mass Spectrometry Conditions are：Using electron impact ion source, trap temperature is 230 DEG C；Chromatography-mass spectroscopy interface temperature is 280 DEG C,
Select ion scan monitoring pattern, quota ion is m/z120.
Testing result is：
Fig. 1 is the selection ion scan chromatogram of n-propyl phthalate standard liquid of the present invention.As can be seen from Figure 1：
The mensure to n-propyl phthalate can be realized using detection method, and retention time is reasonable.
By test method, n-propyl phthalate standard liquid is measured, the results are shown in Table 1.
Table 1：Linear dimensions and detection limit
As known from Table 1, the mass concentration of n-propyl phthalate is linear in the range of 1-10mg/L.
1.0mg/kg is less than by the Monitoring lower-cut (S/N) that signal-to-noise ratio computation obtains method, in addition, by way of mark-on
Detection near analog detection lower limit, the results are shown in Table 2.
Table 2 Monitoring lower-cut experimental result
As known from Table 2, the measurement result near Monitoring lower-cut is accurately and reliably.
By way of mark-on, by test method to sample parallel determination 6 times, the results are shown in Table 3.
Table 3 method repeatability
As known from Table 3, when the present invention detects to sample, repeatability is good, and the RSD% of 6 measurement results is less than
5%.
By test method, mark-on reclaims test is carried out to sample, the results are shown in Table 4.
Table 4
| Compound | Mark-on amount | The rate of recovery |
| N-propyl phthalate | 50mg/kg | 98.9% |
As known from Table 4, n-propyl phthalate is measured by the present invention, it is possible to obtain the comparatively ideal rate of recovery, plus
The mark rate of recovery, between 90-110%, illustrates that method of the present invention accuracy is preferable.
In the above embodiments and its alternative, extracting the solvent using can also be acetone.
In the above embodiments and its alternative, described extraction adopts ultrasonic extraction, and the time of ultrasonic extraction also wraps
Include but be not limited to 3min, 4min, 6min, 7min, 8min, 9min, 10min.
In the above embodiments and its alternative, chromatogram column flow can also for 0.5mL/min, 0.6mL/min,
0.7mL/min、0.8mL/min、0.9mL/min、1.1mL/min、1.2mL/min、1.3mL/min、1.4mL/min、1.5mL/
min、1.6mL/min、1.7mL/min、1.8mL/min、1.9mL/min、2mL/min、2.1mL/min、2.2mL/min、
2.3mL/min、2.4mL/min、2.5mL/min、2.6mL/min、2.7mL/min、2.8mL/min、2.9mL/min、3mL/
min.
In the above embodiments and its alternative, the phenyl of the methyl-polysiloxane of the fixing phase of gas-chromatography
Content can also be 2%, 3%, 4%, 6%, 7%, 8%, 9%, 10%.
In the above embodiments and its alternative, the carrier gas flux of gas-chromatography can also for 0.5mL/min,
0.6mL/min、0.7mL/min、0.8mL/min、0.9mL/min、1.1mL/min、1.2mL/min、1.3mL/min、1.4mL/
min、1.5mL/min、1.6mL/min、1.7mL/min、1.8mL/min、1.9mL/min、2mL/min、2.1mL/min、
2.2mL/min、2.3mL/min、2.4mL/min、2.5mL/min、2.6mL/min、2.7mL/min、2.8mL/min、2.9mL/
min、3mL/min.
In the above embodiments and its alternative, sample injection volume can also be 0.5 μ L, 0.6 μ L, 0.7 μ L, 0.8 μ
L、0.9μL、1.1μL、1.2μL、1.3μL、1.4μL、1.5μL、1.6μL、1.7μL、1.8μL、1.9μL、2μL、2.1μL、2.2μ
L、2.3μL、2.4μL、2.5μL、2.6μL、2.7μL、2.8μL、2.9μL、3μL.
In the above embodiments and its alternative, chromatographic column initial column temperature can also for 130 DEG C, 135 DEG C, 140 DEG C,
145℃、155℃、160℃；Retention time can also be 1min, 1.5min, 2.5min, 3min；Heating rate can also be 5
℃/min、7℃/min、8℃/min、9℃/min、10℃/min；The temperature being warming up to can also for 200 DEG C, 205 DEG C, 210
℃、215℃、220℃、225℃、235℃、240℃、245℃、250℃.Heating rate can also first with 8 DEG C/min, 9 DEG C/
Min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, 15 DEG C/min be warming up to 180 DEG C, 185 DEG C, 190 DEG C, 195
DEG C, 205 DEG C, 210 DEG C, 215 DEG C, 220 DEG C, then with 3 DEG C/min, 4 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min is warming up to
250 DEG C, 251 DEG C, 252 DEG C, 253 DEG C, 254 DEG C, 255 DEG C, 256 DEG C, 257 DEG C, 258 DEG C, 259 DEG C, finally again with 8 DEG C/min, 9
DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, 15 DEG C/min be warming up to 281 DEG C, 285 DEG C, 288 DEG C,
290 DEG C, 293 DEG C, 295 DEG C, 298 DEG C, 300 DEG C, keep 5min, 7min, 8min, 9min, 10min.
In the above embodiments and its alternative, injector temperature can also for 280 DEG C, 285 DEG C, 290 DEG C, 295
℃、305℃、310℃、315℃、320℃.
In the above embodiments and its alternative, trap temperature can also for 200 DEG C, 205 DEG C, 210 DEG C, 215 DEG C,
220℃、225℃、235℃、240℃、245℃、250℃.
In the above embodiments and its alternative, chromatography-mass spectroscopy interface temperature can also for 260 DEG C, 265 DEG C, 270
℃、275℃、280℃、285℃、290℃、295℃.
In the above embodiments and its alternative, quota ion can also for m/z100, m/z 105, m/z 110,
m/z 115、m/z 125、m/z 130、m/z 135、m/z 140、m/z 145、m/z 150.
In view of the present invention program embodiment is numerous, each embodiment experimental data is huge numerous, is not suitable for arranging one by one herein
Lift explanation, but required for each embodiment, the content of checking is all close with the final conclusion obtaining, so unreal to each herein
The checking content applying example is illustrated one by one, only using embodiment 1 as the representative explanation excellent part of the present patent application.
In place of this place embodiment is to the claimed non-limit of technical scope midrange, equally all will in the present invention
Ask in the range of protection.
Specific embodiment described herein is only explanation for example to present invention spirit.The affiliated technology of the present invention is led
The technical staff in domain can be made various modifications or supplement or substituted using similar mode to described specific embodiment, but simultaneously
Do not deviate by the spirit of the present invention or surmount scope defined in appended claims.
Although the present invention has been made a detailed description and has been cited with some specific embodiments, skilled to this area
For technical staff, as long as it is obvious for can making various changes without departing from the spirit and scope of the present invention or revise.
Claims (8)
1. in a kind of articles for washing the detection method of n-propyl phthalate it is characterised in that described detection method is：Join
Make test specimens to be checked, detected using gas chromatography-mass spectrography；
Wherein, GC conditions are：Injector temperature is 280-320 DEG C, and chromatogram column flow is 0.5-3mL/min；Sample enters
Sample amount is 0.5-3 μ L, and chromatographic column initial column temperature is 100-130 DEG C, and after keeping 1-3min, gradient rises to 280-300 DEG C；
Mass Spectrometry Conditions are：Using electron impact ion source, trap temperature is 200-250 DEG C；
Chromatography-mass spectroscopy interface temperature is 260-300 DEG C, selects ion scan monitoring pattern, and quota ion is m/z 100-m/z
150.
2. in a kind of articles for washing according to claim 1 n-propyl phthalate detection method, its feature exists
In the fixing phase of gas-chromatography is methyl-polysiloxane, and wherein the content of phenyl is 2%-10%.
3. in a kind of articles for washing according to claim 1 n-propyl phthalate detection method, its feature exists
In the column length of chromatographic column is 30m, and column internal diameter is 0.25mm.
4. in a kind of articles for washing according to claim 1 n-propyl phthalate detection method, its feature exists
In the gradient increased temperature process of chromatographic column is：First it is warming up to 180-220 DEG C with 8-15 DEG C/min, then be warming up to 3-8 DEG C/min
250-260 DEG C, finally it is warming up to 280-300 DEG C with 8-15 DEG C/min again, keep 5-10min.
5. in a kind of articles for washing according to claim 1 n-propyl phthalate detection method, its feature exists
In the type carrier gases of gas-chromatography are helium, and carrier gas flux is 0.5-3mL/min.
6. in a kind of articles for washing according to claim 1 n-propyl phthalate detection method, its feature exists
In the gasification temperature of gas-chromatography is 250 DEG C.
7. in a kind of articles for washing according to claim 1 n-propyl phthalate detection method, its feature exists
In described trap temperature is 230 DEG C.
8. in a kind of articles for washing according to claim 1 n-propyl phthalate detection method, its feature exists
In described chromatography-mass spectroscopy interface temperature is 280 DEG C.
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| CN201610726042.2A CN106404934A (en) | 2016-08-25 | 2016-08-25 | Method for detecting phthalic acid di-n-propyl ester in washing product |
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| CN201610726042.2A CN106404934A (en) | 2016-08-25 | 2016-08-25 | Method for detecting phthalic acid di-n-propyl ester in washing product |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102721754A (en) * | 2011-03-29 | 2012-10-10 | 王峥涛 | A method for determining phthalate content in traditional Chinese medicine by adopting a liquid chromatography-mass spectrometry method |
| CN104535666A (en) * | 2015-02-11 | 2015-04-22 | 浙江中烟工业有限责任公司 | A method of measuring migration amounts of eighteen phthalic acid esters in a conveyor belt by adopting a gas chromatography-mass spectrometry instrument |
| CN105548394A (en) * | 2015-12-15 | 2016-05-04 | 重庆大学 | Method for supercritical fluid chromatography-based fast separation of phthalate |
-
2016
- 2016-08-25 CN CN201610726042.2A patent/CN106404934A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102721754A (en) * | 2011-03-29 | 2012-10-10 | 王峥涛 | A method for determining phthalate content in traditional Chinese medicine by adopting a liquid chromatography-mass spectrometry method |
| CN104535666A (en) * | 2015-02-11 | 2015-04-22 | 浙江中烟工业有限责任公司 | A method of measuring migration amounts of eighteen phthalic acid esters in a conveyor belt by adopting a gas chromatography-mass spectrometry instrument |
| CN105548394A (en) * | 2015-12-15 | 2016-05-04 | 重庆大学 | Method for supercritical fluid chromatography-based fast separation of phthalate |
Non-Patent Citations (3)
| Title |
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| REN REN 等: "Determination of 17 Phthalate Esters in Infant Milk Powder and Dairy Products by GC–MS with 16 Internal Standards", 《CHROMATOGRAPHIA》 * |
| 周相娟 等: "气相色谱-质谱法测定化妆品中16种邻苯二甲酸酯", 《2010(第十一届)国际表面活性剂和洗涤剂会议论文集》 * |
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