CN106596780B - The method of Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water - Google Patents
The method of Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water Download PDFInfo
- Publication number
- CN106596780B CN106596780B CN201611192699.1A CN201611192699A CN106596780B CN 106596780 B CN106596780 B CN 106596780B CN 201611192699 A CN201611192699 A CN 201611192699A CN 106596780 B CN106596780 B CN 106596780B
- Authority
- CN
- China
- Prior art keywords
- solid
- phase extraction
- extraction column
- water
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
Abstract
Disclosed by the invention is the method for Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water, comprising the following steps: 1) pH of water sample is adjusted；2) solid phase extraction concentration of water sample is concentrated after adjusting pH；3) it is detected using high pressure liquid chromatography-mass spectrograph；4) interpretation of result.The method of Multiple Classes of Antibiotics content has the characteristics that detection time is short, high sensitivity in high pressure liquid chromatography of the invention-mass spectrometry detection water, it is a kind of novel measuring method for Multiple Classes of Antibiotics content in environmental water sample, this method greatly reduces the interference of the detection to object, can carry out simultaneously highly sensitive detection to trace and Multiple Classes of Antibiotics.It is less than 1ppm using the mass accuracy of detection method of the invention for 9 kinds of antibiotic, detection is limited to 0.1-5ug/L, and TIANZHU XINGNAO Capsul 70-100%, relative standard deviation is less than 10%.
Description
Technical field
The present invention relates to technical field of environmental detection, are specifically related to more in high pressure liquid chromatography-mass spectrometry detection water
The method of kind antibiotic content.
Background technique
It is more next that increasingly improve and the newtype drug of the general level of the health constantly put into the dependence that clinical application makes people fight raw element
It is stronger, no matter antibiotic type or quantity be all in increased trend year by year, antibiotic it is a large amount of using inevitably leading
It is caused to enter environment through a variety of ways.Antibiotic in more and more research discovery environment has centainly environmental organism
Toxicity, the antibiotic in environment have been increasingly becoming generally acknowledged emerging pollutant, and the detection to antibiotic in environment has been current
The important content of home and abroad environment detection, improvement and evaluation.
Currently, the detection of antibiotic mainly has gas chromatography, liquid chromatography, gas chromatography-mass spectrometry, liquid phase
Chromatograph-mass spectrometer coupling method.Gas-chromatography and liquid chromatogram rely primarily on chromatography post separation and detector to antibiotic responsiveness, right
Antibiotic detection has preferable qualitatively and quantitatively effect in one pack system or simple system, and since water environment matrix is more multiple
It is miscellaneous, it include gas chromatography matter or interfering ion, there are certain difficulty on antibiotic is qualitative and quantitative for chromatography.Gas-chromatography-
Mass spectrometry and liquid chromatograph mass spectrography mainly utilize chromatography post separation, mass analyzer according to the molecular weight of measurement and
The intensity progress of the Middle Molecular Substance is qualitative and quantitative, and compared with gas-chromatography and liquid chromatogram, chromatography and mass spectrometric hyphenated technique can
Preferably completion complex sample is qualitative and quantitative, however since, there are a large amount of organic matter, background interference is more serious in environment,
The substance classes of identical molecular weight are still very much, so easily causing the false positive of measurement result.
Triple level Four pole technologies are broken into pieces compound molecule, every kind of compound is in certain condition by applying energy
Under have oneself fragments characteristic, compound is carried out by measuring compound molecular weight itself and fragments characteristic molecular weight simultaneously
The qualitative and quantitative erroneous judgement that not only can be reduced to compound reduces false positive and determines, and greatly improves detection sensitivity.At present
The country is less to antibiotic research in high pressure liquid chromatography-mass spectrograph combination method measurement water, is reducing to qualitative and quantitative interference
Cause to pay close attention in environment measuring industry not yet in terms of problem.
Summary of the invention
Present invention solves the technical problem that being to provide a kind of quick, easy, high sensitivity, and effectively reduces or eliminate and
Contain from Multiple Classes of Antibiotics in high pressure liquid chromatography-mass spectrometry detection water of the complex matrices interference antibiotic content in water environment
The method of amount.
The technical scheme is that the method that high pressure liquid chromatography-mass spectrometry detects Multiple Classes of Antibiotics content in water,
The following steps are included:
1) pH of water sample is adjusted: measuring portion 250mL water sample, appropriate formic acid is added, adjust pH to 2.0, another measurement is a
Appropriate ammonium hydroxide is added in 250mL water sample, adjusts pH to 12.0；
2) solid phase extraction concentration of water sample is concentrated after adjusting pH: using 5mL methanol and 10mL deionized water activated solid respectively
Extraction column 1, flow velocity are that the pH 250mL water sample for being adjusted to 2.0 is crossed solid-phase extraction column, flow velocity 3-5mL/ after 5-10mL/min is activated
Min after the excessively complete solid-phase extraction column of water sample, gets solid-phase extraction column express developed with 5mL deionized water, flow velocity 5-10mL/min, so
Solid-phase extraction column 30min is dried afterwards, solid-phase extraction column is finally eluted with 3mL/min flow velocity with 5mL methanol, collects eluent, mark
It is denoted as eluent 1；5mL methanol and 10mL deionized water activated solid extraction column 2 are used respectively, and flow velocity is after 5-10mL/min is activated
The pH 250mL water sample for being adjusted to 12.0 is crossed into solid-phase extraction column, flow velocity 3-5mL/min after the excessively complete solid-phase extraction column of water sample, is used
5mL deionized water gets solid-phase extraction column express developed, then flow velocity 5-10mL/min dries solid-phase extraction column 30min, finally uses
5mL methanol elutes solid-phase extraction column with 3mL/min flow velocity, collects eluent, is labeled as eluent 2；Merge eluent 1 and 2,
It in 40 DEG C of water-baths, is dried with nitrogen with mild, is finally settled to 1mL with water, after 0.45um teflon membrane filter to get arriving
Sample solution；
3) it is detected using high pressure liquid chromatography-mass spectrograph:
A. the preparation of standard solution: accurately weighing standard items antibiotic respectively, using deionized water dissolving, is made into respectively
The Standard Stock solutions of 0.2mg/mL are diluted to standard working solution with deionized water according to the response of each antibiotic when use；
B. high pressure liquid chromatography-mass spectrograph examination criteria working solution and sample solution are used: being inhaled respectively by autosampler
Standard working solution and sample solution are taken, is injected in high pressure liquid chromatography-mass spectrograph, the antibiotic group lease making liquid chromatogram in sample
Post separation, the detection of mass spectrograph multiple-reaction monitoring pattern；
4) data are analyzed: using the parent ion of compound and daughter ion as quota ion and qualitative ion；With standard working solution
Mass concentration X be abscissa, the peak area Y of quantitative and qualitative ion is ordinate, draws standard working curve, is worked with standard
Curve carries out single ion quantified by external standard method to sample；With the chromatographic peak retention time and parent ion/son occurred in sample solution from
Son is qualitative to carrying out.
Further, in the above scheme, formic acid used in the step 1 and ammonium hydroxide are excellent pure grade.
Further, in the above scheme, solid-phase extraction column used in the step 2 is solid for Waters Oasis HLB
Phase extraction column, specification 6cc/500mg, 60um.
Further, in the above scheme, the antibiotic standard items in the step 3 be respectively hygromycin, Lovastatin,
Acarbose, tylosin, erythromycin, sulphadiazine, gentamicin, penicillin, sulfamethoxazole.
Further, in the above scheme, liquid phase chromatogram condition in the step 3: chromatographic column: SB-C18,3.5um, 2.1
×150mm；Mobile phase: A is 0.1% formic acid, and B is acetonitrile；Gradient elution: 0-2min, 10%B；2-7min, 10-40%B, 7-
9min, 40-90%B, 9-10min, 90-100%B；Column temperature: room temperature.
Further, in the above scheme, Mass Spectrometry Conditions in the step 3: mass analyzer: triple level four bars, scanning
Mode: cation-reaction monitoring mode, ion source: electric spray ion source, spray voltage: 4.5kV removes solvent temperature: 500 DEG C,
Remove solvent gas flow velocity: 600L/h.
The beneficial effects of the present invention are: Multiple Classes of Antibiotics contains in high pressure liquid chromatography of the invention-mass spectrometry detection water
The method of amount has the characteristics that detection time is short, high sensitivity, is a kind of novel for Multiple Classes of Antibiotics in environmental water sample
The measuring method of content, this method greatly reduce the interference of the detection to object, can be same to trace and Multiple Classes of Antibiotics
The detection of Shi Jinhang high sensitivity.It is less than 1ppm, inspection using the mass accuracy of detection method of the invention for 9 kinds of antibiotic
Survey is limited to 0.1-5ug/L, and TIANZHU XINGNAO Capsul 70-100%, relative standard deviation is less than 10%.
Detailed description of the invention
Fig. 1 is corresponding multiple-reaction monitoring (MRM) chromatogram of 9 kinds of antibiotic (100 μ g/L).
Specific embodiment
With reference to the accompanying drawing to the side of Multiple Classes of Antibiotics content in high pressure liquid chromatography of the invention-mass spectrometry detection water
Method is described further:
As shown in Figure 1, selection hygromycin, Lovastatin, acarbose, tylosin, erythromycin, sulphadiazine, celebrating are greatly
Mycin, penicillin, sulfamethoxazole carry out a variety of in high pressure liquid chromatography-mass spectrometry detection water as antibiotic standard items
Antibiotic content, specific method the following steps are included:
1) pH of water sample is adjusted: measuring portion 250mL water sample, appropriate formic acid is added, adjust pH to 2.0, another measurement is a
Appropriate ammonium hydroxide is added in 250mL water sample, adjusts pH to 12.0；Formic acid and ammonium hydroxide are excellent pure grade；
2) solid phase extraction concentration of water sample is concentrated after adjusting pH: using 5mL methanol and 10mL deionized water activated solid respectively
Extraction column 1, flow velocity are that the pH 250mL water sample for being adjusted to 2.0 is crossed solid-phase extraction column after 7mL/min activation, flow velocity 4mL/min,
After the excessively complete solid-phase extraction column of water sample, solid-phase extraction column is got express developed with 5mL deionized water, flow velocity 7mL/min is then dry solid
Phase extraction column 30min finally elutes solid-phase extraction column with 5mL methanol with 3mL/min flow velocity, collects eluent, labeled as elution
Liquid 1；5mL methanol and 10mL deionized water activated solid extraction column 2 are used respectively, and flow velocity is to be adjusted to pH after 7mL/min is activated
12.0 250mL water sample crosses solid-phase extraction column, flow velocity 4mL/min, after the excessively complete solid-phase extraction column of water sample, with 5mL deionized water
Get solid-phase extraction column express developed, then flow velocity 7mL/min dries solid-phase extraction column 30min, finally with 5mL methanol with 3mL/
Min flow velocity elutes solid-phase extraction column, collects eluent, is labeled as eluent 2；Above-mentioned solid-phase extraction column used is Waters
Oasis HLB solid-phase extraction column, specification 6cc/500mg, 60um；Merge eluent 1 and 2, in 40 DEG C of water-baths, with mild
Be dried with nitrogen, be finally settled to 1mL with water, after 0.45um teflon membrane filter to get arrive sample solution；
3) it is detected using high pressure liquid chromatography-mass spectrograph:
A. the preparation of standard solution: standard items antibiotic, hygromycin, Lovastatin, acarbose, Thailand are accurately weighed respectively
Happy rhzomorph, erythromycin, sulphadiazine, gentamicin, penicillin, sulfamethoxazole are made into respectively using deionized water dissolving
The Standard Stock solutions of 0.2mg/mL are diluted to standard working solution with deionized water according to the response of each antibiotic when use；
B. high pressure liquid chromatography-mass spectrograph examination criteria working solution and sample solution are used: being inhaled respectively by autosampler
Standard working solution and sample solution are taken, is injected in high pressure liquid chromatography-mass spectrograph, the antibiotic group lease making liquid chromatogram in sample
Post separation, liquid phase chromatogram condition: chromatographic column: SB-C18,3.5um, 2.1 × 150mm；Mobile phase: A is 0.1% formic acid, and B is second
Nitrile；Gradient elution: 0-2min, 10%B；2-7min, 10-40%B, 7-9min, 40-90%B, 9-10min, 90-100%B；Column
Temperature: room temperature；Mass spectrograph multiple-reaction monitoring pattern detection, Mass Spectrometry Conditions: mass analyzer: triple level four bars, scan pattern: just from
Son-reaction monitoring mode, ion source: electric spray ion source, spray voltage: 4.5kV removes solvent temperature: 500 DEG C, removing solvent gas
Body flow velocity: 600L/h；
4) data are analyzed: as shown in table 1, using the parent ion of compound and daughter ion as quota ion and qualitative ion；With
The mass concentration X of standard working solution is abscissa, and the peak area Y of quantitative and qualitative ion is ordinate, draws standard working curve,
Single ion quantified by external standard method is carried out to sample with standard working curve；With the chromatographic peak retention time occurred in sample solution and mother
Ion/daughter ion is qualitative to carrying out, and obtained chromatogram is shown in Fig. 1.
The mass spectrometry parameters of table 1:9 kind antibiotic
| Title | Parent ion/(m/z) | Daughter ion/(m/z) | Orifice potential/V | Collision energy/V |
| Gentamicin | 478.28 | 157.16 | 26 | 20 |
| Lovastatin | 405.16 | 131.35 | 52 | 38 |
| Penicillin | 335.07 | 217.10 | 56 | 16 |
| Sulfamethoxazole | 254.02 | 156.00 | 28 | 16 |
| Sulphadiazine | 251.02 | 155.99 | 24 | 16 |
| Tylosin | 916.55 | 174.12 | 90 | 36 |
| Erythromycin | 734.49 | 158.12 | 44 | 38 |
| Acarbose | 646.28 | 304.19 | 40 | 26 |
| Hygromycin | 528.26 | 177.11 | 52 | 32 |
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment or equivalent replacement of some of the technical features；And
These are modified or replaceed, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (1)
1. the method for Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water, which is characterized in that including following step
It is rapid:
1) pH of water sample is adjusted: portion 250mL water sample is measured, appropriate formic acid is added, adjusts pH to 2.0, it is another to measure portion 250mL
Appropriate ammonium hydroxide is added in water sample, adjusts pH to 12.0；
2) solid phase extraction concentration of water sample is concentrated after adjusting pH: being extracted respectively with 5mL methanol and 10mL deionized water activated solid
Column 1, flow velocity are that the pH 250mL water sample for being adjusted to 2.0 is crossed solid-phase extraction column 1, flow velocity 3-5mL/ after 5-10mL/min is activated
Min after the excessively complete solid-phase extraction column 1 of water sample, gets solid-phase extraction column 1 express developed with 5mL deionized water, flow velocity 5-10mL/min,
Then by the dry 30min of solid-phase extraction column 1, solid-phase extraction column 1 is finally eluted with 3mL/min flow velocity with 5mL methanol, collects elution
Liquid is labeled as eluent 1；5mL methanol and 10mL deionized water activated solid extraction column 2, flow velocity 5-10mL/min are used respectively
The pH 250mL water sample for being adjusted to 12.0 is crossed into solid-phase extraction column 2, flow velocity 3-5mL/min, the excessively complete solid-phase extraction column of water sample after activation
After 2, solid-phase extraction column 2 is got express developed with 5mL deionized water, flow velocity 5-10mL/min is then dry by solid-phase extraction column 2
30min finally elutes solid-phase extraction column 2 with 5mL methanol with 3mL/min flow velocity, collects eluent, is labeled as eluent 2；Merge
Eluent 1 and 2 is dried with nitrogen in 40 DEG C of water-baths with mild, is finally settled to 1mL with water to get sample solution is arrived；
3) it is detected using high pressure liquid chromatography-mass spectrograph:
A. the preparation of standard solution: accurately weighing standard items antibiotic respectively, using deionized water dissolving, is made into 0.2mg/ respectively
The Standard Stock solutions of mL are diluted to standard working solution with deionized water according to the response of each antibiotic when use；
B. high pressure liquid chromatography-mass spectrograph examination criteria working solution and sample solution are used: drawing mark respectively by autosampler
Quasi- working solution and sample solution inject in high pressure liquid chromatography-mass spectrograph, the antibiotic group lease making liquid-phase chromatographic column in sample point
From the detection of mass spectrograph multiple-reaction monitoring pattern；
4) data are analyzed: with parent ion/daughter ion of compound to for quota ion and qualitative ion；With the matter of standard working solution
Amount concentration X is abscissa, and the peak area Y of quantitative and qualitative ion is ordinate, draws standard working curve, uses standard working curve
Single ion quantified by external standard method is carried out to sample；With the chromatographic peak retention time and parent ion/daughter ion pair occurred in sample solution
It carries out qualitative；
Formic acid used in the step 1) and ammonium hydroxide are excellent pure grade；
Solid-phase extraction column 1 used in the step 2) and solid-phase extraction column 2 are Waters Oasis HLB solid-phase extraction column, rule
Lattice are 6cc/500mg, 60 μm；
Antibiotic standard items in the step 3) be respectively hygromycin, Lovastatin, acarbose, tylosin, erythromycin,
Sulphadiazine, gentamicin, penicillin, sulfamethoxazole；
Liquid phase chromatogram condition in the step 3): chromatographic column: SB-C18,3.5 μm, 2.1 × 150mm；Mobile phase: A is 0.1% first
Acid, B are acetonitrile；Gradient elution: 0-2min, 10%B；2-7min, 10-40%B, 7-9min, 40-90%B, 9-10min, 90-
100%B；Column temperature: room temperature；
Mass Spectrometry Conditions in the step 3): mass analyzer: triple level four bars, scan pattern: cation-reaction monitoring mode,
Ion source: electric spray ion source, spray voltage: 4.5kV removes solvent temperature: 500 DEG C, removing solvent gas flow velocity: 600L/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611192699.1A CN106596780B (en) | 2016-12-21 | 2016-12-21 | The method of Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611192699.1A CN106596780B (en) | 2016-12-21 | 2016-12-21 | The method of Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106596780A CN106596780A (en) | 2017-04-26 |
| CN106596780B true CN106596780B (en) | 2019-06-25 |
Family
ID=58602318
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611192699.1A Active CN106596780B (en) | 2016-12-21 | 2016-12-21 | The method of Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106596780B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107941928A (en) * | 2017-10-24 | 2018-04-20 | 东莞市环境监测中心站 | A kind of method of antibiotic in liquid chromatography mass Simultaneous Determination environment water |
| CN108896677A (en) * | 2018-07-17 | 2018-11-27 | 大连职业技术学院 | The method for quickly detecting metrafenone in water using LC-MS technology |
| CN109738565B (en) * | 2019-01-31 | 2021-09-24 | 徐敦明 | Method for determining illegally added compounds in health food |
| CN110133131A (en) * | 2019-05-15 | 2019-08-16 | 上海大学 | The quick determination method of statins in water body |
| CN111707741A (en) * | 2020-06-02 | 2020-09-25 | 南京大学 | Non-target identification method for trace organic pollutant conversion product in environment medium |
| CN115166101A (en) * | 2022-08-04 | 2022-10-11 | 南京理工大学 | Comprehensive screening method for comprehensively identifying new pollutants in water sample |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103293248A (en) * | 2013-06-20 | 2013-09-11 | 中国环境科学研究院 | Method for separating and enriching sulfanilamide antibiotics in water |
| CN104483427A (en) * | 2014-12-08 | 2015-04-01 | 华东理工大学 | Method for separating, enriching and detecting 12 antibiotics in drinking water source |
| CN104990996A (en) * | 2015-05-19 | 2015-10-21 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for detecting antibiotic residues in milk, and application thereof |
| CN105388245A (en) * | 2015-12-25 | 2016-03-09 | 浙江省水产技术推广总站 | Screening method suitable for 46 kinds of medicine in aquatic products |
| CN105548392A (en) * | 2015-12-11 | 2016-05-04 | 中国农业科学院农业资源与农业区划研究所 | Method for simultaneously detecting various antibiotics in livestock and poultry manure by high performance liquid chromatography |
| CN105699537A (en) * | 2016-04-07 | 2016-06-22 | 大连理工大学 | Synchronous detection method for plurality of types of drug residues in water body |
| CN106093220A (en) * | 2016-05-30 | 2016-11-09 | 天津大学 | Detection method while 12 kinds of typical antibiotic in sewage and mud |
-
2016
- 2016-12-21 CN CN201611192699.1A patent/CN106596780B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103293248A (en) * | 2013-06-20 | 2013-09-11 | 中国环境科学研究院 | Method for separating and enriching sulfanilamide antibiotics in water |
| CN104483427A (en) * | 2014-12-08 | 2015-04-01 | 华东理工大学 | Method for separating, enriching and detecting 12 antibiotics in drinking water source |
| CN104990996A (en) * | 2015-05-19 | 2015-10-21 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for detecting antibiotic residues in milk, and application thereof |
| CN105548392A (en) * | 2015-12-11 | 2016-05-04 | 中国农业科学院农业资源与农业区划研究所 | Method for simultaneously detecting various antibiotics in livestock and poultry manure by high performance liquid chromatography |
| CN105388245A (en) * | 2015-12-25 | 2016-03-09 | 浙江省水产技术推广总站 | Screening method suitable for 46 kinds of medicine in aquatic products |
| CN105699537A (en) * | 2016-04-07 | 2016-06-22 | 大连理工大学 | Synchronous detection method for plurality of types of drug residues in water body |
| CN106093220A (en) * | 2016-05-30 | 2016-11-09 | 天津大学 | Detection method while 12 kinds of typical antibiotic in sewage and mud |
Non-Patent Citations (3)
| Title |
|---|
| 固相萃取－液相色谱－串联质谱法测定猪栏废水中10种抗生素;闾幸 等;《理化检验（化学分册）》;20141231;第50卷(第3期);第273-277页 |
| 固相萃取－高效液相色谱－串联质谱法同时测定养殖海水中23种抗生素;杜鹃 等;《色谱》;20150430;第33卷(第4期);第348-353页 |
| 水体中磺胺、四环素、喹诺酮类抗生素检测方法;张俊 等;《中国环境监测》;20130830;第29卷(第4期);第111-115页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106596780A (en) | 2017-04-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106596780B (en) | The method of Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water | |
| Hu | Simultaneous determination of phenylurea herbicides in yam by capillary electrophoresis with electrochemiluminescence detection | |
| Zheng et al. | Evaluating polymer monolith in-tube solid-phase microextraction coupled to liquid chromatography/quadrupole time-of-flight mass spectrometry for reliable quantification and confirmation of quinolone antibacterials in edible animal food | |
| CN105651894B (en) | Method for determining antibiotics in environmental soil | |
| Asiabi et al. | Development of electrochemically controlled packed-in-tube solid phase microextraction method for sensitive analysis of acidic drugs in biological samples | |
| CN102735784A (en) | Method for simultaneously determining one hundred pesticide residuals in traditional Chinese medicine through ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum | |
| CN102353742A (en) | Method for selectively measuring 7 benzene series in white latex for cigarette through static headspace-gas chromatograph mass spectrum | |
| CN111157641B (en) | Method for determining content of carbamazepine in human plasma by HPLC-MS-MS method | |
| CN108318613A (en) | The detection method of antibiotic in a kind of environmental sample | |
| CN110108830B (en) | Method for simultaneously carrying out qualitative and quantitative detection on 9 anthocyanidins in lonicera edulis | |
| CN108896670A (en) | PPCPs pollutant rapid screening detection method in Drinking Water | |
| CN109856285A (en) | Method that is a kind of while detecting multiclass persistent organism in water body | |
| CN109682897A (en) | A kind of method of a variety of incretion interferents in while determination of the environment water sample | |
| CN102798689A (en) | Method for separation enrichment and detection of trace fluoroquinolone antibiotic in water environment | |
| CN107782824A (en) | The quick determination method of a variety of UV stabilizers in a kind of PET bottle | |
| CN105954442A (en) | Method for determining formaldehyde in electronic cigarette liquid | |
| CN105784858B (en) | Method for measuring PPCPs in environmental soil | |
| CN101311718A (en) | Method for determining alkyl quaternaries cation surface active agent by liquid phase chromatography -tandem mass spectrometry combined technology | |
| CN103983707A (en) | Method for detecting drug residues in meat and kit thereof | |
| Li et al. | Determination of deoxynivalenol in cereals by immunoaffinity clean-up and ultra-high performance liquid chromatography tandem mass spectrometry | |
| CN105548431B (en) | Detect the method for oxamyl and oxamyl oxime residual quantity in vegetables/fruit simultaneously | |
| CN102944636B (en) | High-efficiency liquid chromatography to mass spectrum detection method for ethyl carbamate in distilled liquor | |
| Liang et al. | Influence of segmental and selected ion monitoring on quantitation of multi-component using high-pressure liquid chromatography–quadrupole mass spectrometry: simultaneous detection of 16 saponins in rat plasma as a case | |
| CN103472178B (en) | Rapid detecting method for acrylamide content in liquid state seasoning | |
| CN104280473B (en) | The analytical approach of 5 hydroxymethyl furfural in a kind of Linezolid Injection |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |