CN107966507A - Detect the GC-MS methods of dimethyl sulfate ester content in industrial wastes - Google Patents
Detect the GC-MS methods of dimethyl sulfate ester content in industrial wastes Download PDFInfo
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- CN107966507A CN107966507A CN201711170856.3A CN201711170856A CN107966507A CN 107966507 A CN107966507 A CN 107966507A CN 201711170856 A CN201711170856 A CN 201711170856A CN 107966507 A CN107966507 A CN 107966507A
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- -1 dimethyl sulfate ester Chemical class 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title claims abstract description 15
- 239000002440 industrial waste Substances 0.000 title claims abstract description 14
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 34
- 239000012488 sample solution Substances 0.000 claims abstract description 28
- 239000000523 sample Substances 0.000 claims abstract description 19
- 238000001819 mass spectrum Methods 0.000 claims abstract description 6
- 239000012159 carrier gas Substances 0.000 claims abstract description 5
- 239000001307 helium Substances 0.000 claims abstract description 5
- 229910052734 helium Inorganic materials 0.000 claims abstract description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 49
- 239000003085 diluting agent Substances 0.000 claims description 33
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- 150000002500 ions Chemical class 0.000 claims description 12
- 239000012895 dilution Substances 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000010812 external standard method Methods 0.000 claims description 2
- 239000012634 fragment Substances 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000013558 reference substance Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 150000001793 charged compounds Chemical class 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 125000002496 methyl group Chemical class [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
-
- 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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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention discloses a kind of GC MS methods for detecting dimethyl sulfate ester content in industrial wastes, including：(1) configuration standard dimethyl sulfate ester solution, configures sample solution；(2) ion gun used is electron ionization sources, and using 1 chromatographic column of Agilent DB 5MS chromatographic columns or Agilent DB, using helium as carrier gas, using constant current mode, column temperature uses gradient increased temperature pattern, 240 DEG C are risen to from 50 DEG C；(3) the standard dimethyl sulfate ester solution and sample solution difference sample introduction of step (1) are taken, records mass spectrum total ion current figure；(4) concentration of dimethyl suflfate in sample solution is calculated according to the integral area of the concentration of standard dimethyl sulfate ester solution, standard dimethyl sulfate ester solution and sample solution.The method of the present invention uses GC MS analytical technologies, bombards sample by EI ion guns, identifies the presence of dimethyl suflfate by characteristic ion fragment and it is quantified, quick, accurate and high sensitivity.
Description
Technical field
The present invention relates to chemical analysis field, and in particular to the assay method of dimethyl sulfate ester content in a kind of industry waste liquid.
Background technology
Dimethyl suflfate, structure are as follows：
At present, dimethyl suflfate coherent detection report concentrate on air, environment, medicine, surfactant, soil and
Textile etc., the detection method of use have colorimetric method, high performance liquid chromatography, gas chromatography, gas chromatography-mass spectrography
Deng, but each method is in the not Tongfang such as specificity, sensitivity, method precision and repeatability, the operability and convenience of method
Face, all there are it is certain the defects of, it is impossible to reliable quantitative analysis results are provided, and domestic not yet establish sulfuric acid two in industrial wastes
The gas-chromatography of methyl esters-simpleness detection method.
Dimethyl sulfate ester content in industrial wastes is low, meets water unstable, and does not possess UV absorption functional group, accurate fixed
Dimethyl sulfate ester content in amount ground measure industrial wastes is extremely challenging.
The content of the invention
The technical problems to be solved by the invention are, there is provided the gas phase color of dimethyl sulfate ester content in a kind of industrial wastes
Spectrum-mass spectrum (GC-MS) detection method, can measure the content of the dimethyl suflfate in industrial wastes accurate quantitative analysis, have special
One property is good, sensitivity, favorable reproducibility the features such as.
A kind of in order to solve the above technical problems, GC- for detecting dimethyl sulfate ester content in industrial wastes provided by the invention
MS methods, comprise the following steps：
(1) configuration standard dimethyl sulfate ester solution, configures sample solution；
(2) ion gun used is electron ionization sources, using the Agilent DB-5MS (μ of 30m × 0.25mm ID × 0.25
M) chromatographic column or Agilent DB-1 (30m × 0.25mm ID × 0.25 μm) chromatographic column, using helium as carrier gas, using constant current mould
Formula, column temperature use gradient increased temperature pattern, 240 DEG C are risen to from 50 DEG C；
(3) the standard dimethyl sulfate ester solution and sample solution difference sample introduction of step (1) are taken, records mass spectrum total ion current
Figure；
(4) concentration of dimethyl suflfate in sample solution is calculated using external standard method.Can be according to standard dimethyl suflfate
The integral area of the concentration of solution, standard dimethyl sulfate ester solution and sample solution calculates dimethyl suflfate in sample solution
Concentration.
Specifically, the concentration of the standard dimethyl sulfate ester solution is 0.001mg/ml or 0.01mg/mL.
Specifically, the preparation method of the standard dimethyl sulfate ester solution is：Accurately weigh about 50mg dimethyl suflfates extremely
In 10mL volumetric flasks containing 2ml diluents, add diluent constant volume and shake up, precision pipettes the above-mentioned solution of 1mL to 50mL capacity
Bottle, adds diluent constant volume and shakes up, then precision pipettes the solution after the above-mentioned dilutions of 1mL to 100mL volumetric flasks, adds diluent constant volume
And shake up, up to the standard dimethyl sulfate ester solution of about 0.001mg/mL.
Specifically, the preparation method of the standard dimethyl sulfate ester solution is：Accurately weigh about 50mg dimethyl suflfates extremely
In 10mL volumetric flasks containing 2ml diluents, add diluent constant volume and shake up, precision pipettes the above-mentioned solution of 1mL to 50mL capacity
Bottle, adds diluent constant volume and shakes up, then precision pipettes the solution after the above-mentioned dilutions of 1mL to 10mL volumetric flasks, adds diluent constant volume
And shake up, up to the standard dimethyl sulfate ester solution of about 0.01mg/mL.
Specifically, the sample solution is industrial wastes sample, diluent is added to be settled to the sample solution of about 100mg/mL.
Specifically, the diluent is chromatographic grade acetonitrile.
Specifically, the characteristic peak that fragment ion molecular weight is 95 and 96 is extracted in GC-MS detection methods.
Specifically, the flow velocity under the constant current mode is 0.65ml/min.
Specifically, the detailed process of the gradient increased temperature is：Initial temperature is 50 DEG C；120 DEG C are warming up to 10 DEG C/min,
120 DEG C of holding 2min；240 DEG C are warming up to 30 DEG C/min, and keeps 5min.
Specifically, take 1 μ L sample introductions of sample solution.
Specifically, it is 10 that split ratio is set in GC-MS detection methods：1.
The method of the present invention uses GC-MS analytical technologies, sample is bombarded by EI ion guns, so as to produce electronics and molecule
Ion, molecular ion continue to be subject to electron bombardment and cause the fracture moment of chemical bond to produce different kinds of ions, pass through characteristic ion
Fragment identifies the presence of dimethyl suflfate and it quantified, quick, accurate and high sensitivity.
Brief description of the drawings
Fig. 1 is the mass spectrum rod figure for the dimethyl suflfate that the embodiment of the present invention 1 obtains.
Fig. 2 is the compares figure for the dimethyl suflfate that the embodiment of the present invention 1 obtains.
Fig. 3 is the sample detection figure that the embodiment of the present invention 1 obtains.
Fig. 4 is the compares figure for the dimethyl suflfate that the embodiment of the present invention 2 obtains.
Fig. 5 is the sample detection figure that the embodiment of the present invention 2 obtains.
Fig. 6 is the specificity figure that the embodiment of the present invention 3 obtains.
Fig. 7 is the quantitative limit figure that the embodiment of the present invention 3 obtains.
Embodiment
Clear, complete description is carried out to technical scheme below in conjunction with attached drawing, it is clear that described implementation
Example is the part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this area
Art personnel all other embodiments obtained on the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
Embodiment 1
Instrument and condition：
Gas chromatography-mass spectrometry：Agilent 7890B GC, 5977A MS detectors
Chromatographic column：Agilent DB-5MS(30m×0.25mm ID×0.25μm)
Ion gun：Electron ionization sources
Carrier gas：Helium
Solvent delay：4.5min
Pattern：Constant current
Flow velocity：0.65ml/min
Split ratio：10：1
Sample size：1μL
Extract molecular weight：95 and 96；
Injector temperature：200℃
Column temperature gradient is as follows：
| Ramp | Temperature | Hold Time |
| - | 50℃ | 0min |
| 10℃/min | 120℃ | 2min |
| 30℃/min | 240℃ | 5min |
Experimental procedure：
Diluent：Acetonitrile.
Standard dimethyl sulfate ester solution：The accurate about 50mg dimethyl suflfates that weigh are to the 10mL capacity containing 2ml diluents
In bottle, adding diluent constant volume and shake up, precision pipettes the above-mentioned solution of 1mL to 50mL volumetric flasks, adds diluent constant volume and shakes up, then
Precision pipettes the solution after the above-mentioned dilutions of 1mL to 10mL volumetric flasks, adds diluent constant volume and shakes up, up to about 0.01mg/mL's
Standard dimethyl sulfate ester solution.
Sample solution：It is accurate to weigh in about 1g sample solutions to the 10mL volumetric flasks containing 2ml diluents, add diluent to determine
Hold and shake up, up to the sample solution of about 100mg/mL.
Mass spectrum rod figure is recorded, sees Fig. 1.Compares figure is recorded, sees Fig. 2, standard dimethyl sulfate ester solution is at RT7.813min
Appearance.Sample drawing is recorded, sees Fig. 3, sample solution is not detected by dimethyl suflfate appearance, illustrates this reality again at same retention time
Apply in the industrial wastewater sample of example and do not detect dimethyl suflfate, meet emission request.
Embodiment 2
Instrument and condition：
Gas chromatography-mass spectrometry：Agilent 7890B GC, 5977A MS detectors
Chromatographic column：Agilent DB-1(30m×0.25mm ID×0.25μm)
Ion gun：Electron ionization sources
Carrier gas：Helium
Solvent delay：4.5min
Pattern：Constant current
Flow velocity：0.65ml/min
Split ratio：10：1
Sample size：1μL
Extract molecular weight：95 and 96；
Injector temperature：200℃
Column temperature gradient is as follows：
| Ramp | Temperature | Hold Time |
| - | 50℃ | 0min |
| 10℃/min | 120℃ | 2min |
| 30℃/min | 240℃ | 5min |
Experimental procedure：
Diluent：Acetonitrile.
Standard dimethyl sulfate ester solution：The accurate about 50mg dimethyl suflfates that weigh are to the 10mL capacity containing 2ml diluents
In bottle, adding diluent constant volume and shake up, precision pipettes the above-mentioned solution of 1mL to 50mL volumetric flasks, adds diluent constant volume and shakes up, then
Precision pipettes the solution after the above-mentioned dilutions of 1mL to 100mL volumetric flasks, adds diluent constant volume and shakes up, up to about 0.001mg/mL
Standard dimethyl sulfate ester solution.
Sample solution：It is accurate to weigh in about 1g sample solutions to the 10mL volumetric flasks containing 2ml diluents, add diluent to determine
Hold and shake up, up to the sample solution of about 100mg/mL.
Compares figure is recorded, sees Fig. 4, standard dimethyl sulfate ester solution appearance at RT7.632min.Sample drawing is recorded, sees figure
5, sample solution detects dimethyl suflfate appearance at same retention time, and detected level is less than quantitative limit 5ppm.
Embodiment 3：Methodology validation
1. specificity is tested
Take dimethyl suflfate reference substance appropriate, according to the method for example 2, prepare standard dimethyl sulfate ester solution, and should
Solution is detected analysis according to the method for example 2 using gas chromatography mass spectrometry.
Test result indicates that at dimethyl suflfate retention time, blank is noiseless；Dimethyl suflfate tailing factor
0.93, peak type is good；For dimethyl suflfate peak separating degree adjacent thereto up to 6.65, separating degree is good.It is specifically shown in Fig. 6.
2. quantitative limit is tested
Take dimethyl suflfate reference substance appropriate, according to the method for example 2, prepare standard dimethyl sulfate ester solution, precision is moved
The above-mentioned solution of 5mL is taken to add diluent constant volume to 10mL volumetric flasks and shake up, the solution is used gas phase according to the method for example 2
Chromatographic mass spectrometry method is detected analysis.
Test result indicates that when dimethyl sulfate ester concentration reaches 0.0005mg/mL, the ratio of main peak peak height and baseline noise
Up to 52.60, sensitivity is good.It is specifically shown in Fig. 7.
3. linearity and range
Take dimethyl suflfate reference substance appropriate, it is accurately weighed, dissolved with diluent and diluted successively, concentration range is made and exists
The series standard solution of 0.0005mg/mL~0.005mg/mL.And each standard solution is used into gas phase color according to the method for example 2
Spectrum mass spectrography is detected analysis, records chromatogram, and using concentration as abscissa, peak area is ordinate, carries out linear regression, and
Regression equation and related coefficient are calculated, the results are shown in Table 1.
The linearity and range experimental result of 1 dimethyl suflfate of table
Test result indicates that in the range of 0.0005mg/mL~0.005mg/mL, dimethyl suflfate is linearly good.
4. Precision Experiment
Take dimethyl suflfate reference substance appropriate, according to the method for example 2, prepare standard dimethyl sulfate ester solution, and should
Solution is detected analysis according to the method for example 2 using gas chromatography mass spectrometry, continuous sample introduction 3 times, record retention time and
Peak area, and result is evaluated, it the results are shown in Table 2.
2 system Precision test result of table
| Inserting needle number | 1 | 2 | 3 | Average | RSD% |
| Peak area | 3575 | 3782 | 3727 | 3695 | 2.90% |
| Retention time (min) | 7.632 | 7.631 | 7.632 | 7.632 | 0.01% |
Test result indicates that method precision is good.
5. stability experiment
Take dimethyl suflfate reference substance appropriate, according to the method for example 2, prepare standard dimethyl sulfate ester solution；It is accurate to claim
Take in about 1g sample solutions (industrial wastes) to the 10mL volumetric flasks containing 2ml standard dimethyl sulfate ester solutions, the quasi- sulfuric acid of mark-on
Diformazan ester solution constant volume simultaneously shakes up, up to the sample mark-on solution (rate of recovery solution) of about 100mg/mL, as study on the stability
Solution, and the solution is detected analysis according to the method for example 2 using gas chromatography mass spectrometry, respectively at 0,5,7,14,
19,24 it is small when injecting chromatograph, record retention time and peak area, and result is evaluated, the results are shown in Table 3.
3 stability experiment result of table
| Sample injection time (h) | 0 | 5 | 7 | 14 | 19 | 24 | Average | RSD% |
| Peak area | 3831 | 4119 | 4310 | 4506 | 4763 | 4714 | 4374 | 8.23% |
| Retention time (min) | 7.63 | 7.636 | 7.638 | 7.652 | 7.653 | 7.693 | 7.650 | 0.30% |
Test result indicates that dimethyl suflfate at least 24h in diluent acetonitrile stablizes, have good stability.
6. the rate of recovery is tested
Take dimethyl suflfate reference substance appropriate, according to the method for example 2, prepare standard dimethyl sulfate ester solution；It is accurate to claim
Take in about 1g sample solutions (industrial wastes) to the 10mL volumetric flasks containing 2ml standard dimethyl sulfate ester solutions, the quasi- sulfuric acid of mark-on
Diformazan ester solution constant volume simultaneously shakes up, parallel to prepare two parts up to the rate of recovery solution of about 100mg/mL, and by each solution according to reality
The method of example 2 is detected analysis using gas chromatography mass spectrometry, the results are shown in Table 4.
4 rate of recovery experimental result of table
Test result indicates that the dimethyl suflfate rate of recovery is good.
In conclusion the various embodiments described above and attached drawing are only presently preferred embodiments of the present invention, not limiting this
The protection domain of invention, within the spirit and principles of the invention, any modification, equivalent substitution, improvement and etc. done, all should
Comprising within the scope of the present invention.
Claims (10)
- A kind of 1. GC-MS methods for detecting dimethyl sulfate ester content in industrial wastes, it is characterised in that including：(1) configuration standard dimethyl sulfate ester solution, configures sample solution；(2) ion gun used is electron ionization sources, using Agilent DB-5MS chromatographic columns or Agilent DB-1 chromatographic columns, Using helium as carrier gas, using constant current mode, column temperature uses gradient increased temperature pattern, 240 DEG C is risen to from 50 DEG C；(3) the standard dimethyl sulfate ester solution and sample solution difference sample introduction of step (1) are taken, records mass spectrum total ion current figure；(4) concentration of dimethyl suflfate in sample solution is calculated using external standard method.
- 2. the method as described in claim 1, it is characterised in that the concentration of the standard dimethyl sulfate ester solution is 0.001mg/ ml。
- 3. method as claimed in claim 2, it is characterised in that the preparation method of the standard dimethyl sulfate ester solution is：It is accurate Really weigh in about 50mg dimethyl suflfates to the 10mL volumetric flasks containing 2ml diluents, add diluent constant volume and shake up, precision is moved The above-mentioned solution of 1mL is taken to add diluent constant volume to 50mL volumetric flasks and shake up, then the solution that precision is pipetted after the above-mentioned dilutions of 1mL arrives 100mL volumetric flasks, add diluent constant volume and shake up, up to the standard dimethyl sulfate ester solution of about 0.001mg/mL.
- 4. the method as described in claim 1, it is characterised in that the sample solution is industrial wastes sample, adds diluent to determine Hold to the sample solution of about 100mg/mL.
- 5. the method as described in claim 3 or 4, it is characterised in that the diluent is chromatographic grade acetonitrile.
- 6. the method as described in claim 1, it is characterised in that the characteristic peak that extraction fragment ion molecular weight is 95 and 96.
- 7. the method as described in claim 1, it is characterised in that the flow velocity under the constant current mode is 0.65ml/min.
- 8. the method as described in claim 1, it is characterised in that the detailed process of the gradient increased temperature is：Initial temperature is 50 ℃；120 DEG C are warming up to 10 DEG C/min, 120 DEG C of holding 2min；240 DEG C are warming up to 30 DEG C/min, and keeps 5min.
- 9. the method as described in claim 1, it is characterised in that take 1 μ L sample introductions of sample solution.
- 10. the method as described in claim 1, it is characterised in that it is 10 to set split ratio：1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111579689A (en) * | 2020-06-11 | 2020-08-25 | 江苏联环药业股份有限公司 | Method for measuring content of dimethyl sulfate in clopidogrel hydrogen sulfate |
| CN112858507A (en) * | 2021-01-12 | 2021-05-28 | 苏州国辰生物科技股份有限公司 | Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry |
| CN113640425A (en) * | 2021-08-23 | 2021-11-12 | 宜昌人福药业有限责任公司 | Method for detecting content of dimethyl sulfate in sulfamethoxazole bulk drug |
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Cited By (3)
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| CN111579689A (en) * | 2020-06-11 | 2020-08-25 | 江苏联环药业股份有限公司 | Method for measuring content of dimethyl sulfate in clopidogrel hydrogen sulfate |
| CN112858507A (en) * | 2021-01-12 | 2021-05-28 | 苏州国辰生物科技股份有限公司 | Analysis method for measuring dimethyl sulfate in pyraclostrobin by gas chromatography-mass spectrometry |
| CN113640425A (en) * | 2021-08-23 | 2021-11-12 | 宜昌人福药业有限责任公司 | Method for detecting content of dimethyl sulfate in sulfamethoxazole bulk drug |
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