CN105548408A - Method for detecting caprolactam in chinlon textile - Google Patents
Method for detecting caprolactam in chinlon textile Download PDFInfo
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- CN105548408A CN105548408A CN201610059149.6A CN201610059149A CN105548408A CN 105548408 A CN105548408 A CN 105548408A CN 201610059149 A CN201610059149 A CN 201610059149A CN 105548408 A CN105548408 A CN 105548408A
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- caprolactam
- polyamide fibre
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a method for detecting caprolactam in a chinlon textile. The method comprises the following steps: treating the chinlon textile to obtain chinlon textile fragments; weighing a certain quantity of the chinlon textile fragments, adding secondary distilled water, and performing constant-temperature treatment in a drying oven of 80-120 DEG C for 45-90 minutes; performing ultrasonic treatment in an ultrasonic cleaner for 20-50 minutes, taking the fragments out, cooling to the room temperature, shaking uniformly, filtering, extracting supernatant liquid, and filtering through a water-borne filtering film to obtain liquid to be detected; and detecting the content of the chinlon textile in the liquid to be detected by adopting an ultra-high performance liquid chromatography triple quadrupole gas chromatograph-mass spectrometer. According to the method, distilled water ultrasonic extraction is adopted, so that a sample treatment process is simplified, the cost is lowered, and the detection efficiency is increased; a detection limit is 40mumg/kg, which is 10-20 times lower than that of the conventional caprolactam detection method, and the detection demand of future ecological textiles can be met.
Description
Technical field
The present invention relates to the detection method of caprolactam, particularly relate to the detection method of caprolactam in polyamide fibre textile.
Background technology
Polyamide fibre, formal name used at school Silon, be China produce the general designation of polyamide-based fiber.Claim nylon in the world.Intensity is high, wearing quality, occupies first of all fibres.Its wearing quality is 10 times of cotton fiber, is 10 times of dry state viscose rayon, is 140 times of hygrometric state fiber, purely can spins and make various dress material and knit goods with blending.The kind of polyamide fibre is a lot, has polyamide fibre 6, polyamide fibre 66, polyamide fibre 11, polyamide fibre 610 wherein most importantly polyamide fibre 66 and polyamide fibre 6.The character of various polyamide fibre is incomplete same, and common feature macromolecular main chain has acid amides chain, can adsorbed water molecule, and can form crystalline texture, anti-wear performance is very excellent, is all excellent clothing fiber.
Caprolactam is one of important industrial chemicals, mainly for the production of nylon-6 fiber and polyamide, can be processed into synthon further, engineering plastics, food contact material etc.
Caprolactam has spread effect to the eyes of human body and nervous centralis, particularly to brain stem, parenchymal viscera can be caused to damage, human contact's caprolactam can cause bitter taste nose to stimulate the symptoms such as gastric disorder, can absorb through skin, dry skin furfur severe patient of chapping can be caused can to cause general dermatitis.Long Term Contact can cause gene mutation and then destroy chromosome.
In addition, caprolactam physics and chemistry character is comparatively stable, is difficult to degraded, at the highest limitation≤15mg/kg of GB/T6332-1996 National Standard of the People's Republic of China food containers, wrappage nylon molding product hygienic standard regulation caprolactam.
Less for the method measuring caprolactam in polyamide fibre textile, in having been reported, major part is all adopt the method for high performance liquid chromatography ultraviolet coupling to measure, and small part adopts vapor-phase chromatography to measure.These two kinds of methods all have certain limitation, when adopting high performance liquid chromatography ultraviolet combination analysis, are easily subject to the spectra1 interfer-of impurity and matrix, produce false positive erroneous judgement.Adopt vapor-phase chromatography analysis to analyze, baseline fluctuates greatly, and noise is high, detects limit for height, detecting device specific aim difference and respond and sensitivity low.Therefore, further investigation measures caprolactam necessary containing the new method of content in polyamide fibre textile.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, provide a kind of by force targeted, detection limit is low, and Detection results is good, analyzes consuming time short, the detection method of caprolactam in the polyamide fibre textile that levels of precision is high.
The present invention is achieved by the following technical solutions:
In polyamide fibre textile, the detection method of caprolactam, comprises the steps:
S1, polyamide fibre textile treatment is obtained polyamide fibre textile fragment;
S2, take a certain amount of polyamide fibre textile fragment, add redistilled water, constant temperature process 45-90min in the baking oven of 80-120 DEG C;
S3, in ultrasonic cleaner ultrasonic process 20-50min, be cooled to room temperature after taking-up, after shaking up filtration, get supernatant liquor;
S4, by S3 product by water system membrane filtration, obtain liquid to be measured;
S5, employing Ultra Performance Liquid Chromatography triple level Four bar GC-MS measure the content of caprolactam in the liquid to be measured of S4.
The liquid chromatography optimum configurations of described Ultra Performance Liquid Chromatography triple level Four bar GC-MS is as follows:
Column temperature: 20-40 DEG C;
Sampling volume: 1-5uL;
Mobile phase: A methyl alcohol, B water;
Flow velocity: 0.4mL/min;
Deng degree analysis: A=65%, B=35%;
Analysis time: 4min.
The mass spectrometry parameters of described Ultra Performance Liquid Chromatography triple level Four bar GC-MS arranges as follows:
Ionization mode: positive ion mode, ESI ion gun;
Dry gas temperature: 350 DEG C;
Dry gas flow velocity: 10L/min;
Nebulizer pressure: 45psi;
Capillary voltage: 4000V;
Scan mode: multiple-reaction monitoring, parent ion m/z114, quota ion m/z55, qualitative ion m/z44, m/z43, m/z69;
Cracked voltage: 123eV;
Impact energy: m/z55 is 25eV; M/z44 is 29eV; M/z43 is 21eV; M/z69 is 17eV.
Preferably, in described step S2, the mass ratio of polyamide fibre textile fragment and redistilled water is 1:18-24.
Preferably, in described step S2, the mass ratio of polyamide fibre textile fragment and redistilled water is 1:20.
Preferably, in described step S2, the temperature of baking oven is 100 DEG C, and the time of constant temperature process is 60min.
Preferably, in described step S3, the time of ultrasonic process is 30min.
Preferably, in described step S4, the aperture of water system filter membrane is 0.22-1.20um.
Preferably, in described step S4, the aperture of water system filter membrane is 0.23um.
The invention has the beneficial effects as follows:
(1) adopt distilled water ultrasonic extraction in the present invention, compared with traditional soxhlet extraction, the consumption of solvent obviously reduces, non-toxic to operating personnel in distilled water extraction process, and the time obviously shorten, simplify the processing procedure of sample, reduce cost, improve detection efficiency;
(2) adopt Ultra Performance Liquid Chromatography triple level Four bar GC-MS in the present invention, greatly can get rid of the interference of matrix and impurity;
(3) the present invention is by carrying out exploration optimization to the operating conditions of Ultra Performance Liquid Chromatography triple level Four bar GC-MS, and test result is more accurate, and precision is high, favorable reproducibility;
(4) of the present invention detecting is limited to 40ug/kg, and lower than the detection limit of existing caprolactam method of testing 10-20 times, lower detection limit can adapt to the detection demand of following ecological textile.
Accompanying drawing explanation
In order to be illustrated more clearly in technical scheme of the present invention, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only embodiments of the invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the chromatogram of the caprolactam standard items of 4ug/L in embodiments of the invention 1;
Fig. 2 is the chromatogram of the caprolactam detected in embodiments of the invention 1;
Fig. 3 is the mass spectrogram of the caprolactam detected in embodiments of the invention 1;
Fig. 4 is the typical curve of the caprolactam detected in embodiments of the invention 1;
Fig. 5 be in embodiments of the invention 2 liquid to be measured chromatogram;
Fig. 6 be in embodiments of the invention 3 liquid to be measured chromatogram;
Fig. 7 be in embodiments of the invention 4 liquid to be measured chromatogram;
Fig. 8 be in embodiments of the invention 5 liquid to be measured chromatogram.
Embodiment
Below in conjunction with the accompanying drawing in the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite of not making creative work, all belongs to the scope of protection of the invention.
The optimum configurations of the Ultra Performance Liquid Chromatography that following examples adopt triple level Four bar GC-MS is as follows:
Adopt ZORBAXEclipsePlusC18 chromatographic column, column length 50mm, internal diameter 3.0, particle diameter 1.8um;
Column temperature: 20-40 DEG C;
Sampling volume: 1-5uL;
Mobile phase: A methyl alcohol B water, analysis such as degree of grade: A=65%, B=35%;
Flow velocity: 0.4mL/min;
Analysis time: 4min;
Ionization mode: positive ion mode, ESI ion gun;
Dry gas temperature: 350 DEG C;
Dry gas flow velocity: 10L/min;
Nebulizer pressure: 45psi;
Capillary voltage: 4000V;
Scan mode: multiple-reaction monitoring, parent ion m/z114, quota ion m/z44, qualitative ion m/z55, m/z43, m/z69;
Cracked voltage: 123eV;
Impact energy: m/z55 is 25eV; M/z44 is 29eV; M/z43 is 21eV; M/z69 is 17eV.
Wherein, column temperature and sampling volume are variable element, and other parameters immobilize.
Below in conjunction with embodiment and accompanying drawing 1-8, illustrate the present invention further.
Embodiment 1:
Refer to Fig. 1-4.The invention discloses the drafting of caprolactam standard working curve, use ten thousand/ electronic balance take the volumetric flask that 0.0817g caprolactam standard items (purity is 98%) are placed in 100mL, dissolve with methyl alcohol and be settled to scale mark, shake up, preparation concentration is the caprolactam storing solution of 800mg/L; Then pipette 1000uL caprolactam storing solution in the volumetric flask of 100mL, by methanol constant volume to scale mark, shake up, obtain the caprolactam intermediate liquid that concentration is 8mg/L; Pipette 50uL respectively, 100uL, 200uL, the caprolactam intermediate liquid of 500uL, 1000uL in 5 100mL volumetric flasks, by methanol constant volume to scale mark, shake up, obtain the caprolactam titer that concentration is 4ug/L, 8ug/L, 16ug/L, 40ug/L, 80ug/L.
Detect above-mentioned titer by Ultra Performance Liquid Chromatography triple level Four bar GC-MS, the column temperature of Ultra Performance Liquid Chromatography triple level Four bar GC-MS is set to 25 DEG C, and sampling volume is set to 2uL.
With quota ion (m/z44) chromatographic peak area for ordinate, with the concentration of titer for horizontal ordinate drawing standard curve.
The linear equation of typical curve is Y=33.299986X+32.223606, and related coefficient is R2=0.9999, linearly well, can be used for the detection of caprolactam.
Embodiment 2:
Refer to Fig. 5.The invention discloses the detection method of caprolactam in woman style sweater (acrylic 72.7%, polyamide fibre 27.3%), choose above-mentioned polyamide fibre textile, manually shred, and mix.Choose the sample of 2mm*2mm size, precision takes the sample shredded of 1.0g, is accurate to 0.0001g, be placed in 40ml reaction tube, adding 20.0ml redistilled water, constant temperature 1 hour in 100 DEG C of baking ovens, is ultrasonic process 30min in the ultrasonic cleaning machine of 40kHz subsequently in frequency, to be cooled to room temperature after taking out, shake up up and down, be filtered in clean extracting tube, use needle injector supernatant liquor, cross 0.23um water system filter membrane, obtain liquid to be measured.
Repeat the preparation process 3 times of above-mentioned liquid to be measured, obtain the Duplicate Samples A of 3 increment product liquid to be measured, B, C.
Detect above-mentioned 3 parts of Duplicate Samples by Ultra Performance Liquid Chromatography triple level Four bar GC-MS, the column temperature of Ultra Performance Liquid Chromatography triple level Four bar GC-MS is set to 25 DEG C, and sampling volume is set to 2uL.Typical curve in the peak area corresponding according to quota ion and example 1 draws the concentration of sample testing liquid, and calculate content (mg/kg) mean value and the relative standard deviation RSD of caprolactam in woman style sweater further, test result is in table 1.
Table 1:
To Duplicate Samples A replication 5 times, the results are shown in Table 2.
Table 2:
Embodiment 3:
Refer to Fig. 6.The invention discloses the detection method of caprolactam content in super soft polyamide fibre one trousers (dacron 56.1%, polyamide fibre 31%, spandex 12.9%), choose above-mentioned polyamide fibre textile, manually shred, and mix.Choose the sample of 2mm*2mm size, precision takes the sample shredded of 1.0g, is accurate to 0.0001g, be placed in 40ml reaction tube, adding 18.0ml redistilled water, constant temperature 90min in 80 DEG C of baking ovens, is ultrasonic process 20min in the ultrasonic cleaning machine of 40kHz subsequently in frequency, to be cooled to room temperature after taking out, shake up up and down, be filtered in clean extracting tube, use needle injector supernatant liquor, cross 0.22um water system filter membrane, obtain liquid to be measured.
Repeat the preparation process 3 times of above-mentioned liquid to be measured, obtain the Duplicate Samples A of 3 increment product liquid to be measured, B, C.
Detect above-mentioned 3 parts of Duplicate Samples by Ultra Performance Liquid Chromatography triple level Four bar GC-MS, the column temperature of Ultra Performance Liquid Chromatography triple level Four bar GC-MS is set to 20 DEG C, and sampling volume is set to 1uL.Typical curve in the peak area corresponding according to quota ion and example 1 draws the concentration of sample testing liquid, calculate content (mg/kg) mean value and the relative standard deviation RSD of caprolactam in excess of export soft polyamide fibre one trousers further, test result is in table 3.
Table 3:
To Duplicate Samples A replication 5 times, the results are shown in Table 4.
Table 4:
Embodiment 4:
Refer to Fig. 7.The invention discloses the detection method of caprolactam content in woman style sweater (polyamide fibre 100%), choose above-mentioned woman style sweater, manually shred, and mix.Choose the sample of 2mm*2mm size, precision takes the sample shredded of 1.0g, is accurate to 0.0001g, be placed in 40ml reaction tube, adding 24.0ml redistilled water, constant temperature 45min in 120 DEG C of baking ovens, is ultrasonic process 50min in the ultrasonic cleaning machine of 40kHz subsequently in frequency, to be cooled to room temperature after taking out, shake up up and down, be filtered in clean extracting tube, use needle injector supernatant liquor, cross 1.20um water system filter membrane, obtain liquid to be measured.
Repeat the preparation process 3 times of above-mentioned liquid to be measured, obtain the Duplicate Samples A of 3 increment product liquid to be measured, B, C.
Detect above-mentioned 3 parts of Duplicate Samples by Ultra Performance Liquid Chromatography triple level Four bar GC-MS, the column temperature of Ultra Performance Liquid Chromatography triple level Four bar GC-MS is set to 40 DEG C, and sampling volume is set to 5uL.Typical curve in the peak area corresponding according to quota ion and example 1 draws the concentration of sample testing liquid, and calculate content (mg/kg) mean value and the relative standard deviation RSD of caprolactam in woman style sweater further, test result is in table 5.
Table 5:
To Duplicate Samples A replication 5 times, the results are shown in Table 6.
Table 6:
Embodiment 5:
Refer to Fig. 8.The invention discloses the detection method of caprolactam content in lady's underwear (polyamide fibre 84%, spandex 16%), choose certain brand lady's underwear above-mentioned, manually shred, and mix.Choose the sample of 2mm*2mm size, precision takes the sample shredded of 1.0g, is accurate to 0.0001g, be placed in 40ml reaction tube, adding 20.0ml redistilled water, constant temperature 1 hour in 100 DEG C of baking ovens, is ultrasonic process 30min in the ultrasonic cleaning machine of 40kHz subsequently in frequency, to be cooled to room temperature after taking out, shake up up and down, be filtered in clean extracting tube, use needle injector supernatant liquor, cross 0.23um water system filter membrane, obtain liquid to be measured.
Repeat the preparation process 3 times of above-mentioned liquid to be measured, obtain the Duplicate Samples A of 3 increment product liquid to be measured, B, C.
Detect above-mentioned 3 parts of Duplicate Samples by Ultra Performance Liquid Chromatography triple level Four bar GC-MS, the column temperature of Ultra Performance Liquid Chromatography triple level Four bar GC-MS is set to 30 DEG C, and sampling volume is set to 3uL.Typical curve in the peak area corresponding according to quota ion and example 1 draws the concentration of sample testing liquid, and calculate content (mg/kg) mean value and the relative standard deviation RSD of caprolactam in lady's underwear further, test result is in table 7.
Table 7:
To Duplicate Samples A replication 5 times, the results are shown in Table 8.
Table 8:
Embodiment 6:
The invention discloses a kind of method of testing of the caprolactam recovery, standard solution in embodiment 1 is joined in the liquid to be measured of ready known negative result (after tested not containing target compound), test according to embodiment 1 Instrumental analyzing detecting method, the column temperature of Ultra Performance Liquid Chromatography triple level Four bar GC-MS is set to 25 DEG C, and sampling volume is set to 2uL.Do 6 horizontal surveies to this liquid to be measured to average, according to actual addition and measured result, calculate the recovery of standard addition of this liquid to be measured, the results are shown in Table 9.
Table 9:
The calculating of method detection limit: when the signal to noise ratio (S/N ratio) (S/N) of target peak reaches 3, the concentration of caprolactam is 2ug/L, and namely instrument detection limit is 2ug/L, and method detects and is limited to 40ug/kg.
Data from table 1 to table 9, the detection method of caprolactam in polyamide fibre textile of the present invention, detect and be limited to 40ug/kg, the recovery is between 92.20%-106.03%, RSD is between 0.89%-5.41%, visible, in above-mentioned polyamide fibre textile, the detection method of caprolactam has higher sensitivity, accuracy and precision.
The invention has the beneficial effects as follows:
(1) adopt distilled water ultrasonic extraction in the present invention, compared with traditional soxhlet extraction, the consumption of solvent obviously reduces, non-toxic to operating personnel in distilled water extraction process, and the time obviously shorten, simplify the processing procedure of sample, reduce cost, improve detection efficiency;
(2) adopt Ultra Performance Liquid Chromatography triple level Four bar GC-MS in the present invention, greatly can get rid of the interference of matrix and impurity;
(3) the present invention is by carrying out exploration optimization to the operating conditions of Ultra Performance Liquid Chromatography triple level Four bar GC-MS, and test result is more accurate, and precision is high, favorable reproducibility;
(4) of the present invention detecting is limited to 40ug/kg, and lower than the detection limit of existing caprolactam method of testing 10-20 times, lower detection limit can adapt to the detection demand of following ecological textile.
The above is the preferred embodiment of the present invention; it is noted that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (9)
1. the detection method of caprolactam in polyamide fibre textile, is characterized in that, comprise the steps:
S1, polyamide fibre textile treatment is obtained polyamide fibre textile fragment;
S2, take a certain amount of polyamide fibre textile fragment, add redistilled water, constant temperature process 45-90min in the baking oven of 80-120 DEG C;
S3, in ultrasonic cleaner ultrasonic process 20-50min, be cooled to room temperature after taking-up, after shaking up filtration, get supernatant liquor;
S4, by S3 product by water system membrane filtration, obtain liquid to be measured;
S5, employing Ultra Performance Liquid Chromatography triple level Four bar GC-MS measure the content of caprolactam in the liquid to be measured of S4.
2. the detection method of caprolactam in polyamide fibre textile according to claim 1, it is characterized in that, the liquid chromatography optimum configurations of described Ultra Performance Liquid Chromatography triple level Four bar GC-MS is as follows:
Column temperature: 20-40 DEG C;
Sampling volume: 1-5uL;
Mobile phase: A methyl alcohol, B water;
Flow velocity: 0.4mL/min;
Deng degree analysis: A=65%, B=35%;
Analysis time: 4min.
3. the detection method of caprolactam in polyamide fibre textile according to claim 1 and 2, it is characterized in that, the mass spectrometry parameters of described Ultra Performance Liquid Chromatography triple level Four bar GC-MS arranges as follows:
Ionization mode: positive ion mode, ESI ion gun;
Dry gas temperature: 350 DEG C;
Dry gas flow velocity: 10L/min;
Nebulizer pressure: 45psi;
Capillary voltage: 4000V;
Scan mode: multiple-reaction monitoring, parent ion m/z114, quota ion m/z55, qualitative ion m/z44, m/z43, m/z69;
Cracked voltage: 123eV;
Impact energy: m/z55 is 25eV; M/z44 is 29eV; M/z43 is 21eV; M/z69 is 17eV.
4. the detection method of caprolactam in polyamide fibre textile according to claim 1, it is characterized in that, in described step S2, the mass ratio of polyamide fibre textile fragment and redistilled water is 1:18-24.
5. the detection method of caprolactam in polyamide fibre textile according to claim 4, it is characterized in that, in described step S2, the mass ratio of polyamide fibre textile fragment and redistilled water is 1:20.
6. in the polyamide fibre textile according to claim 1 or 4, the detection method of caprolactam, is characterized in that, in described step S2, the temperature of baking oven is 100 DEG C, and the time of constant temperature process is 60min.
7. the detection method of caprolactam in polyamide fibre textile according to claim 1, it is characterized in that, the time of ultrasonic process in described step S3 is 30min.
8. the detection method of caprolactam in polyamide fibre textile according to claim 1, it is characterized in that, in described step S4, the aperture of water system filter membrane is 0.22-1.20um.
9. the detection method of caprolactam in polyamide fibre textile according to claim 8, it is characterized in that, in described step S4, the aperture of water system filter membrane is 0.23um.
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| CN107894481A (en) * | 2018-01-11 | 2018-04-10 | 南通市食品药品监督检验中心 | A kind of method of caprolactam in ultra-performance liquid chromatography measure food contact material nylon 6 |
| CN110895267A (en) * | 2019-11-29 | 2020-03-20 | 福建永荣科技有限公司 | Method for determining caprolactam content in ammonium sulfate by high performance liquid chromatography |
| CN111122720A (en) * | 2019-12-11 | 2020-05-08 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | High performance liquid chromatography analysis method of caprolactam, 6-aminocaproamide and 6-aminocapronitrile |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107894481A (en) * | 2018-01-11 | 2018-04-10 | 南通市食品药品监督检验中心 | A kind of method of caprolactam in ultra-performance liquid chromatography measure food contact material nylon 6 |
| CN110895267A (en) * | 2019-11-29 | 2020-03-20 | 福建永荣科技有限公司 | Method for determining caprolactam content in ammonium sulfate by high performance liquid chromatography |
| CN111122720A (en) * | 2019-12-11 | 2020-05-08 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | High performance liquid chromatography analysis method of caprolactam, 6-aminocaproamide and 6-aminocapronitrile |
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