CN109142568A - A method of utilizing gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids - Google Patents
A method of utilizing gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids Download PDFInfo
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- CN109142568A CN109142568A CN201810912818.9A CN201810912818A CN109142568A CN 109142568 A CN109142568 A CN 109142568A CN 201810912818 A CN201810912818 A CN 201810912818A CN 109142568 A CN109142568 A CN 109142568A
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Abstract
The present invention relates to technical field of food detection, especially a kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids.Solid phase extraction techniques are additionally used in the present invention in addition to extracting to sample, have chosen the molecular blotting column that can purify grease, grease can be effectively removed by being handled by oil sample；The present invention reduces detection limit by two kinds of approach, first is that sample is concentrated, such as weigh 10g sample, finally object is concentrated in 0.5ml solvent, concentrates 20 times, method detection limit can be reduced, second is that being detected using Gas-phase acidity instrument, its detector is mass spectrum, and detection limit reaches 1ppb, greatly reduces method detection limit.
Description
Technical field
The present invention relates to technical field of food detection, especially a kind of to utilize gas chromatograph-mass spectrometer (GC-MS) quantitative detection
The method of Capsaicinoids.
Background technique
Capsaicine constituent structure is more stable, easily remains in gutter oil, is not easy to remove in gutter oil process, just
Capsaicine is not contained in normal edible oil, therefore capsaicine can be used as the important evidence for identifying gutter oil.Existing capsaicine inspection
Survey technology mainly uses GB/T 21266-2007 and NY/T 1381-2007 method, efficient liquid phase detection, and method detection limit is
130ppb, detection limit is higher, and being unable to reach the requirement that food safety country risk monitors, (the maximum of capsaicine is limited the quantity in peanut oil
≤ 4ppb), and simple organic solvent extracts the lubricant component being difficult to remove in matrix, if directly upper machine testing, to instrument
It damages larger.In " measurement of capsaicine in edible oil and fat " of the publication of on 2 24th, 2018 Food and drug administration general bureaus, food is mended
It fills and uses LC-MS instrument in the method for inspection, but the more difficult popularization and application of equipment price valuableness.Therefore need to develop one kind preceding
The influence of matrix grease can be effectively removed when processing, detecting instrument has good sensitivity, while instrument equipment valence again
The cheap capsaicine detection method of lattice.
Summary of the invention
The purpose of the present invention is to provide a kind of using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids
Method overcomes aforementioned the deficiencies in the prior art, and sample pre-treatments can effectively remove grease, and detection limit reaches 1ppb,
Meet country risk testing requirements.
The technical scheme adopted by the invention to solve the technical problem is that: it is a kind of fixed using gas chromatograph-mass spectrometer (GC-MS)
The method of amount detection Capsaicinoids, includes the following steps:
(1) oil sample pre-treatment: weighing 8-15g oil sample, and the acetonitrile of 10-30ml n-hexane saturation is added in oil sample, then uses
Turbine mixer vortex 1-3min, with ultrasonic washing instrument ultrasound 20-50min, centrifuge is centrifuged 3-10min, takes supernatant, then
The acetonitrile of 10-30ml n-hexane saturation is added, repeats said extracted step 2 time, collects the supernatant after extracting 3 times, will collect
To supernatant be placed in chicken heart bottle；
(2) it is concentrated: the chicken heart bottle for filling supernatant in step (1) being placed in Rotary Evaporators, by chicken heart bottle at 30-40 DEG C
Rotary evaporated to dryness, point 3 n-hexane redissolution being saturated every time with 3ml acetonitrile, the solution obtained after redissolution are collected in glass tube
In；
(3) purification elution: the solution being collected in glass tube in step (2) is activated with molecular blotting column, after activation again
Extracting solution is purified with molecular blotting column, is eluted after purification with 3-10ml acetonitrile, eluent is collected, uses nitrogen at 35-45 DEG C
The dry instrument drying of air-blowing；
(4) machine testing on: the acetonitrile solution 0.3-1ml of the eluent after being dried with nitrogen in step (3) is redissolved, upper machine testing.
Preferably, a method of using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids, including it is as follows
Step:
(1) oil sample pre-treatment: weighing 10g oil sample, and the acetonitrile of 15ml n-hexane saturation is added in oil sample, then mixed using being vortexed
Clutch vortex 2min, with ultrasonic washing instrument ultrasound 30min, centrifuge is centrifuged 5min, takes supernatant, add 15ml n-hexane
The acetonitrile of saturation repeats said extracted step 2 time, collects the supernatant after extracting 3 times, the supernatant being collected into is placed in heart
In bottle；
(2) it is concentrated: the chicken heart bottle for filling supernatant in step (1) being placed in Rotary Evaporators, is revolved chicken heart bottle at 35 DEG C
Turn to be evaporated to dryness, point 3 n-hexanes for using 3ml acetonitrile to be saturated every time redissolve, and the solution obtained after redissolution is collected in glass tube；
(3) purification elution: the solution being collected in glass tube in step (2) is activated with molecular blotting column, after activation again
Extracting solution is purified with molecular blotting column, is eluted after purification with 5ml acetonitrile, eluent is collected, with being dried with nitrogen at 40 DEG C
Instrument drying；
(4) machine testing on: the acetonitrile solution 0.5ml of the eluent after being dried with nitrogen in step (3) is redissolved, using gas phase color
Machine testing in spectrum-mass spectrometer.
Preferably, in the step (4), the temperature program of gas chromatograph-mass spectrometer (GC-MS) are as follows: 55-65 DEG C of sample introduction is protected
1-3 min is held, 15-25 DEG C/min is warming up to 210 DEG C, keeps 1-2 min, then be warming up to 300 DEG C with 12-18 DEG C/min, protects
Hold 3-7 min.
Preferably, in the step (4), the temperature program of gas chromatograph-mass spectrometer (GC-MS) are as follows: 60 DEG C of sample introductions keep 2
Min, 20 DEG C/min are warming up to 210 DEG C, keep 1 min, then be warming up to 300 DEG C with 15 DEG C/min, keep 5 min.
Preferably, the chromatographic column of the gas chromatograph-mass spectrometer (GC-MS) is DM-5MS.
Preferably, input mode is not shunt when the gas chromatograph-mass spectrometer (GC-MS) use, injector temperature 285
DEG C, 290 DEG C of transmission line temperature, 300 DEG C of ion source temperature.
Preferably, the mass spectrometry parameters of the gas chromatograph-mass spectrometer (GC-MS) are as follows: the qualitative ion of capsaicine: capsaicine is qualitative
Ion is 138,152, quota ion 137；The qualitative ion of internal standard compound is 171,283, quota ion 153.
It is of the invention a kind of to utilize gas chromatograph-mass spectrometer (GC-MS) the beneficial effects of the present invention are: compared with prior art
The method of quantitative detection Capsaicinoids has the advantages that (1) can effectively remove grease by oil sample pre-treatment,
Solid phase extraction techniques are additionally used in the present invention in addition to extracting to sample, have chosen the molecular blotting column that can purify grease；
(2) greatly reduce method detection limit: the present invention reduces detection limit by two kinds of approach, first is that sample is concentrated, such as
10g sample is weighed, finally object is concentrated in 0.5ml solvent, concentrates 20 times, method detection limit can be reduced, second is that
It is detected using Gas-phase acidity instrument, detector is mass spectrum, and detection limit reaches 1ppb.
Detailed description of the invention
Fig. 1 is natural capsicum element correlation spectrogram of the present invention；
Fig. 2 is Dihydrocapsaicin correlation spectrogram of the present invention；
Fig. 3 is internal standard compound total ion current figure of the present invention；
Fig. 4 is natural capsicum quality spectrogram of the present invention；
Fig. 5 is Dihydrocapsaicin mass spectrogram of the present invention
Fig. 6 is internal standard substance spectrogram of the present invention；
Fig. 7 is signal-to-noise ratio figure of the present invention.
Specific embodiment
A kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids of embodiment 1
The present embodiment agents useful for same: the general grade n-hexane of color, chromatographic grade acetonitrile, chromatographic grade methylene chloride (be used for molecular blotting column),
Natural capsicum element standard items, Dihydrocapsaicin standard items, the own ester (D4-DEHP) of internal standard compound D4- phthalic acid two (2- ethyl).
The present embodiment instrument consumptive material: gas chromatograph-mass spectrometer (GC-MS), assay balance, turbine mixer, ultrasonic cleaning
Instrument, Rotary Evaporators, is dried with nitrogen instrument, chicken heart bottle, volumetric flask, molecular blotting column, disposable centrifuge tube at centrifuge.
This fact Example blank sample is the peanut oil without capsaicine of our company's production, and the day of 1ng/ml is added thereto
The Dihydrocapsaicin of right capsaicine and 1ng/ml, is made the oil sample of the present embodiment.
A method of utilizing gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids, comprising the following steps:
(1) oil sample pre-treatment: weighing 10g oil sample, and the acetonitrile of 15ml n-hexane saturation is added in oil sample, then mixed using being vortexed
Clutch vortex 2min, with ultrasonic washing instrument ultrasound 30min, centrifuge is centrifuged 5min, takes supernatant, add 15ml n-hexane
The acetonitrile of saturation repeats said extracted step 2 time, collects the supernatant after extracting 3 times, the supernatant being collected into is placed in heart
In bottle；
(2) it is concentrated: the chicken heart bottle for filling supernatant in step (1) being placed in Rotary Evaporators, is revolved chicken heart bottle at 35 DEG C
Turn to be evaporated to dryness, point 3 n-hexane redissolution being saturated with 3ml acetonitrile, the solution obtained after redissolution is collected in glass tube；
(3) purification elution: the solution being collected in glass tube in step (2) is activated with molecular blotting column, after activation again
Extracting solution is purified with molecular blotting column, is eluted after purification with 5ml acetonitrile, eluent is collected, with being dried with nitrogen at 40 DEG C
Instrument drying；
(4) machine testing on: the acetonitrile solution 0.5ml of the eluent after being dried with nitrogen in step (3) is redissolved, using gas phase color
Machine testing in spectrum-mass spectrometer.
A kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids of embodiment 2
The present embodiment agents useful for same: the general grade n-hexane of color, chromatographic grade acetonitrile, chromatographic grade methylene chloride (be used for molecular blotting column),
Natural capsicum element standard items, Dihydrocapsaicin standard items, the own ester (D4-DEHP) of internal standard compound D4- phthalic acid two (2- ethyl).
The present embodiment instrument consumptive material: gas chromatograph-mass spectrometer (GC-MS), assay balance, turbine mixer, ultrasonic cleaning
Instrument, Rotary Evaporators, is dried with nitrogen instrument, chicken heart bottle, volumetric flask, molecular blotting column, disposable centrifuge tube at centrifuge.
This fact Example blank sample is the peanut oil without capsaicine of our company's production, and the day of 2ng/ml is added thereto
The Dihydrocapsaicin of right capsaicine and 2ng/ml, is made the oil sample of the present embodiment.
A method of utilizing gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids, comprising the following steps:
(1) oil sample pre-treatment: weighing 10g oil sample, and the acetonitrile of 15ml n-hexane saturation is added in oil sample, then mixed using being vortexed
Clutch vortex 2min, with ultrasonic washing instrument ultrasound 30min, centrifuge is centrifuged 5min, takes supernatant, add 15ml n-hexane
The acetonitrile of saturation repeats said extracted step 2 time, collects the supernatant after extracting 3 times, the supernatant being collected into is placed in heart
In bottle；
(2) it is concentrated: the chicken heart bottle for filling supernatant in step (1) being placed in Rotary Evaporators, is revolved chicken heart bottle at 35 DEG C
Turn to be evaporated to dryness, point 3 n-hexane redissolution being saturated with 3ml acetonitrile, the solution obtained after redissolution is collected in glass tube；
(3) purification elution: the solution being collected in glass tube in step (2) is activated with molecular blotting column, after activation again
Extracting solution is purified with molecular blotting column, is eluted after purification with 5ml acetonitrile, eluent is collected, with being dried with nitrogen at 40 DEG C
Instrument drying；
(4) machine testing on: the acetonitrile solution 0.5ml of the eluent after being dried with nitrogen in step (3) is redissolved, using gas phase color
Machine testing in spectrum-mass spectrometer.
A kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids of embodiment 3
The present embodiment agents useful for same: the general grade n-hexane of color, chromatographic grade acetonitrile, chromatographic grade methylene chloride (be used for molecular blotting column),
Natural capsicum element standard items, Dihydrocapsaicin standard items, the own ester (D4-DEHP) of internal standard compound D4- phthalic acid two (2- ethyl).
The present embodiment instrument consumptive material: gas chromatograph-mass spectrometer (GC-MS), assay balance, turbine mixer, ultrasonic cleaning
Instrument, Rotary Evaporators, is dried with nitrogen instrument, chicken heart bottle, volumetric flask, molecular blotting column, disposable centrifuge tube at centrifuge.
This fact Example blank sample is the peanut oil without capsaicine of our company's production, and the day of 4ng/ml is added thereto
The Dihydrocapsaicin of right capsaicine and 4ng/ml, is made the oil sample of the present embodiment.
A method of utilizing gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids, comprising the following steps:
(1) oil sample pre-treatment: weighing 10g oil sample, and the acetonitrile of 15ml n-hexane saturation is added in oil sample, then mixed using being vortexed
Clutch vortex 2min, with ultrasonic washing instrument ultrasound 30min, centrifuge is centrifuged 5min, takes supernatant, add 15ml n-hexane
The acetonitrile of saturation repeats said extracted step 2 time, collects the supernatant after extracting 3 times, the supernatant being collected into is placed in heart
In bottle；
(2) it is concentrated: the chicken heart bottle for filling supernatant in step (1) being placed in Rotary Evaporators, is revolved chicken heart bottle at 35 DEG C
Turn to be evaporated to dryness, point 3 n-hexane redissolution being saturated with 3ml acetonitrile, the solution obtained after redissolution is collected in glass tube；
(3) purification elution: the solution being collected in glass tube in step (2) is activated with molecular blotting column, after activation again
Extracting solution is purified with molecular blotting column, is eluted after purification with 5ml acetonitrile, eluent is collected, with being dried with nitrogen at 40 DEG C
Instrument drying；
(4) machine testing on: the acetonitrile solution 0.5ml of the eluent after being dried with nitrogen in step (3) is redissolved, using gas phase color
Machine testing in spectrum-mass spectrometer.
The test of 1 result of experimental example
Using inner mark method ration, internal standard or external standard analysis method are established according to equipment operation, standard curve is established and is determined
Amount calculates.
Standard curve correlation: natural capsicum element: R > 0.99, Dihydrocapsaicin: R > 0.99.
In embodiment 1-3, using a kind of utilization gas chromatograph-mass spectrometer (GC-MS) quantitative detection capsaicine class object of the invention
The method of matter, the recovery of standard addition data detected are as shown in table 1:
Table 1
It can be seen that out the rate of recovery between 90-110% from the data in table 1.
Relative standard deviation data are as shown in table 2:
The data of table 2 can be seen that out blank sample mark-on 1ppb relative standard deviation≤10%.
Natural capsicum element correlation spectrogram is as shown in Figure 1, as can be seen from the figure correlation is 0.9981；Dihydrocapsaicin
Correlation spectrogram is as shown in Fig. 2, as can be seen from the figure correlation is 0.9982；Internal standard compound total ion current figure as shown in figure 3, from
It can be seen that internal standard compound peak row is good in figure, RSD value is 7.9；Natural capsicum quality spectrogram is as shown in figure 4, can from figure
Qualitatively and quantitatively ion is 137,138,152 out；Dihydrocapsaicin mass spectrogram as shown in figure 5, it is as can be seen from the figure quantitative and
Qualitative ion is 137,138,152；Internal standard substance spectrogram as shown in fig. 6, as can be seen from the figure internal standard compound qualitatively and quantitatively from
Son is 153,171,283；Signal-to-noise ratio figure is as shown in fig. 7, can be seen that sample mark-on 1ppb, signal-to-noise ratio S/N from signal-to-noise ratio spectrogram
About 68 times, 3 times of the signal-to-noise ratio greater than standard requirements is detection limit, and the method detection limit can be set to 1ppb.
Above-mentioned specific embodiment is only specific case of the invention, and scope of patent protection of the invention includes but is not limited to
The product form and style of above-mentioned specific embodiment, any claims of the present invention and any technical field of meeting
The appropriate changes or modifications that those of ordinary skill does it, all shall fall within the protection scope of the present invention.
Claims (7)
1. a kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids, it is characterised in that: including such as
Lower step:
Oil sample pre-treatment: weighing 8-15g oil sample, and the acetonitrile of 10-30ml n-hexane saturation is added in oil sample, then using vortex
Mixer vortex 1-3min, with ultrasonic washing instrument ultrasound 20-50min, centrifuge is centrifuged 3-10min, takes supernatant, add
The acetonitrile of 10-30ml n-hexane saturation, repeats said extracted step 2 time, the supernatant after extracting is collected 3 times, by what is be collected into
Supernatant is placed in chicken heart bottle；
Concentration: the chicken heart bottle for filling supernatant in step (1) is placed in Rotary Evaporators, is revolved chicken heart bottle at 30-40 DEG C
Turn to be evaporated to dryness, point 3 n-hexanes for using 3ml acetonitrile to be saturated every time redissolve, and the solution obtained after redissolution is collected in glass tube；
Purification elution: the solution being collected in glass tube in step (2) is activated with molecular blotting column, is used and is divided again after activation
Sub- trace column purifies extracting solution, is eluted after purification with 3-10ml acetonitrile, collects eluent, is blown at 35-45 DEG C with nitrogen
Dry instrument drying；
Upper machine testing: the acetonitrile solution 0.3-1ml of the eluent after being dried with nitrogen in step (3) is redissolved, upper machine testing.
2. a kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids as described in claim 1,
It is characterized by comprising following steps:
(1) oil sample pre-treatment: weighing 10g oil sample, and the acetonitrile of 15ml n-hexane saturation is added in oil sample, then mixed using being vortexed
Clutch vortex 2min, with ultrasonic washing instrument ultrasound 30min, centrifuge is centrifuged 5min, takes supernatant, add 15ml n-hexane
The acetonitrile of saturation repeats said extracted step 2 time, collects the supernatant after extracting 3 times, the supernatant being collected into is placed in heart
In bottle；
(2) it is concentrated: the chicken heart bottle for filling supernatant in step (1) being placed in Rotary Evaporators, is revolved chicken heart bottle at 35 DEG C
Turn to be evaporated to dryness, point 3 n-hexanes for using 3ml acetonitrile to be saturated every time redissolve, and the solution obtained after redissolution is collected in glass tube；
(3) purification elution: the solution being collected in glass tube in step (2) is activated with molecular blotting column, after activation again
Extracting solution is purified with molecular blotting column, is eluted after purification with 5ml acetonitrile, eluent is collected, with being dried with nitrogen at 40 DEG C
Instrument drying；
(4) machine testing on: the acetonitrile solution 0.5ml of the eluent after being dried with nitrogen in step (3) is redissolved, using gas phase color
Machine testing in spectrum-mass spectrometer.
3. a kind of side using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids as claimed in claim 1 or 2
Method, it is characterised in that: in the step (4), the temperature program of gas chromatograph-mass spectrometer (GC-MS) are as follows: 55-65 DEG C of sample introduction is kept
1-3 min, 15-25 DEG C/min are warming up to 210 DEG C, keep 1-2 min, then be warming up to 300 DEG C with 12-18 DEG C/min, keep
3-7 min。
4. a kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids as claimed in claim 3,
It is characterized by: in the step (4), the temperature program of gas chromatograph-mass spectrometer (GC-MS) are as follows: 60 DEG C of sample introductions keep 2 min,
20 DEG C/min is warming up to 210 DEG C, keeps 1 min, then be warming up to 300 DEG C with 15 DEG C/min, keeps 5 min.
5. a kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids as claimed in claim 4,
It is characterized by: the chromatographic column of the gas chromatograph-mass spectrometer (GC-MS) is DM-5MS.
6. a kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids as claimed in claim 4,
It is characterized by: input mode is not shunt when the gas chromatograph-mass spectrometer (GC-MS) use, injector temperature is 285 DEG C, is passed
290 DEG C of defeated line temperature, 300 DEG C of ion source temperature.
7. a kind of method using gas chromatograph-mass spectrometer (GC-MS) quantitative detection Capsaicinoids as claimed in claim 4,
It is characterized by: the mass spectrometry parameters of the gas chromatograph-mass spectrometer (GC-MS) are as follows: the qualitative ion of capsaicine is 138,152, it is quantitative from
Son is 137；The qualitative ion of internal standard compound is 171,283, quota ion 153.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090102136A (en) * | 2008-03-25 | 2009-09-30 | 주식회사 내츄로바이오텍 | Compositions for controlling nematodes and eggs comprising plant extracts as effective components |
| CN102680608A (en) * | 2012-06-13 | 2012-09-19 | 中国广州分析测试中心 | Method for identifying abandoned kitchen oil |
| CN105911195A (en) * | 2016-04-06 | 2016-08-31 | 中国计量科学研究院 | Preparation method for edible oil standard substance containing capsicine compound |
| CN105963352A (en) * | 2016-06-15 | 2016-09-28 | 江苏康缘药业股份有限公司 | Cinnamon oil and application of main ingredient cinnamaldehyde of cinnamon oil |
-
2018
- 2018-08-10 CN CN201810912818.9A patent/CN109142568A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090102136A (en) * | 2008-03-25 | 2009-09-30 | 주식회사 내츄로바이오텍 | Compositions for controlling nematodes and eggs comprising plant extracts as effective components |
| CN102680608A (en) * | 2012-06-13 | 2012-09-19 | 中国广州分析测试中心 | Method for identifying abandoned kitchen oil |
| CN105911195A (en) * | 2016-04-06 | 2016-08-31 | 中国计量科学研究院 | Preparation method for edible oil standard substance containing capsicine compound |
| CN105963352A (en) * | 2016-06-15 | 2016-09-28 | 江苏康缘药业股份有限公司 | Cinnamon oil and application of main ingredient cinnamaldehyde of cinnamon oil |
Non-Patent Citations (7)
| Title |
|---|
| PENA-ALVAREZ,ARACELI 等: "Analysis of capsaicin and dihydrocapsaicin in peppers and pepper sauces by solid phase microextraction–gas chromatography–mass spectrometry", 《INSTRUMENTATION SCIENCE & TECHNOLOGY》 * |
| 刘百战 等: "辣椒油化学成分的气相色谱-质谱分析", 《分析测试学报》 * |
| 吴惠勤 等: "LC-MS/MS鉴别地沟油新方法", 《分析测试学报》 * |
| 孙汉巨 等: "《食品分析与检测实验》", 31 December 2016, 合肥工业大学出版社 * |
| 赵琴 等: "固相萃取-超高效液相色谱-串联质谱快速检测食用油和地沟油中辣椒素和二氢辣椒素", 《分析科学学报》 * |
| 赵田甜 等: "气相色谱串联质谱法测定个人护理产品中的4种发热剂", 《现代化工》 * |
| 齐文启 等: "《痕量有机污染物的监测》", 31 December 2001, 化学工业出版社 * |
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