CN109212109B - High performance liquid chromatography-mass spectrometry determination method for iprodione in tobacco and tobacco products - Google Patents
High performance liquid chromatography-mass spectrometry determination method for iprodione in tobacco and tobacco products Download PDFInfo
- Publication number
- CN109212109B CN109212109B CN201811429923.3A CN201811429923A CN109212109B CN 109212109 B CN109212109 B CN 109212109B CN 201811429923 A CN201811429923 A CN 201811429923A CN 109212109 B CN109212109 B CN 109212109B
- Authority
- CN
- China
- Prior art keywords
- iprodione
- sample
- tobacco
- standard
- liquid chromatography
- 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
Images
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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
-
- 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
A high performance liquid chromatography-mass spectrometry method for iprodione in tobacco and tobacco products is characterized in that: decomposing all the iprodione in the sample into metabolites [ iprodione de- (N-isopropyl formamide) ] by using an alkaline solution, acidifying by using hydrochloric acid, performing liquid-liquid extraction by using dichloromethane, filtering, blowing nitrogen to be nearly dry, re-dissolving by using acetonitrile, and measuring the content of the iprodione metabolites in the sample by using liquid chromatography-mass spectrometry so as to indirectly measure the total amount of the iprodione in the sample. The method overcomes the defects of the sample treatment method in the prior art, fills the blank of the measurement of the substances, can provide a plurality of references for the measurement of related residual limit and the development of method technology, optimizes the sample pretreatment method and the instrument detection conditions aiming at the tobacco sample, and has the following excellent effects compared with the prior art: the method has the advantages of simple and quick sample pretreatment process, accurate operation, high sensitivity and good repeatability.
Description
Technical Field
The invention belongs to the technical field of physicochemical inspection of pesticide residues in tobacco products, and mainly relates to a determination technology of the residual quantity of iprodione in tobacco, in particular to a method for determining the content of iprodione in a sample by decomposing the iprodione in the sample into metabolites [ iprodione de- (N-isopropyl formamide) ] by using an alkaline solution, extracting the metabolites with dichloromethane liquid after acidification, filtering the products, and determining the content of the iprodione metabolites in the sample by using liquid chromatography-mass spectrometry, thereby indirectly determining the content of the iprodione in the sample.
Background
The pesticide residue of tobacco as smoking product is an important component of the safety problem of smoking, and the pesticide residue index of tobacco and tobacco products is an important content in the quality control of tobacco products in various countries, is an important factor for the evaluation and purchase of tobacco leaves in international market, and is also an important content for commodity inspection in the international trade of tobacco. Iprodione, also known as prochloraz, belongs to the dicarboximide class and is a broad-spectrum contact-killing type protective bactericide. The bactericide has influence on various development stages in the life history of pathogenic fungi, and is widely used for disease control of fruit trees, vegetables and grains and storage and preservation of fruits. Is suitable for preventing and treating vegetable and fruit diseases such as tomato gray mold, early blight, apple alternaria leaf spot and the like by leaf surface spraying. Currently, the MRL (maximum residual limit) values of iprodione on tobacco, cucumber and tomato established in China are 0.1, 2.0 and 5.0 mg/kg, respectively. At present, GC-MS, HPLC and HPLC-MS methods are mostly adopted for detecting the residual quantity of iprodione, and pretreatment methods mainly comprise liquid-liquid extraction, solid-phase extraction and matrix dispersion solid-phase extraction. In the methods, iprodione is taken as a detection object, but the iprodione is easily decomposed in a sample to generate iprodione de- (N-isopropyl formamide) [ Chinese agronomy report, 2017,33: 150-. The measurement method of the present invention is proposed based on this.
The invention content is as follows:
the invention aims to overcome the defects of the prior art by aiming at the current situations of complex tobacco matrix conditions, various samples and the like, and provides a method for directly measuring the residual quantity of iprodione metabolites in tobacco products by liquid chromatography-mass spectrometry by combining liquid-liquid extraction with a matrix matching method, thereby indirectly measuring the content of iprodione in the samples. The method can quickly and accurately detect the total amount of iprodione residues in the tobacco, and has accurate determination result and less determination interference.
The mechanism of the invention is that the iprodione in the sample is completely converted into the iprodione de- (N-isopropyl formamide) in the alkaline environment, the total amount of the iprodione in the sample is indirectly measured by measuring the content of the iprodione de- (N-isopropyl formamide), the method is simple and convenient, and a new thought is provided for measuring the residual amount of the iprodione in the tobacco.
The purpose of the invention is realized by the following technical scheme:
a high-performance liquid chromatography-mass spectrometry method for measuring iprodione in tobacco and tobacco products comprises decomposing all iprodione in a sample into its metabolite, namely iprodione de- (N-isopropyl formamide), acidifying with hydrochloric acid, extracting with dichloromethane liquid, filtering, blowing nitrogen to near dryness, redissolving with acetonitrile, and measuring the content of iprodione metabolite in the sample by liquid chromatography-mass spectrometry, thereby indirectly measuring the content of iprodione in the sample. The method specifically comprises the following steps:
a. and (3) extracting a sample: accurately weigh 1.0 g of sample (to the nearest 0.01 g) into a 50 mL centrifuge tube with a lid. 18 mL of 0.2 moL/L sodium hydroxide solution was added, and the tube was placed on a vortex mixer shaker and shaken at 2000 rpm for 2 min. Then placing in a water bath kettle at 90 deg.C for 30 min. Cooling to room temperature, adding 2.0 mL of hydrochloric acid solution with the mass fraction of 30%, mixing uniformly, adding 10 mL of dichloromethane, and oscillating at the speed of 2000 rpm for 2 min. Sucking 1mL of lower layer clear liquid, blowing nitrogen to be nearly dry, re-dissolving with 1.0 mL of acetonitrile, filtering by a 0.45-micron organic phase filter membrane, and detecting by LC-MS;
b. preparation of standard working solution: respectively weighing 10 mg (accurate to 0.1 mg) of iprodione metabolite standard substance in a 10 mL volumetric flask, selecting acetonitrile to dissolve according to the solubility of the standard substance, and fixing the volume to scale to prepare a first-level standard stock solution. And transferring 1.0 mL of standard stock solution into a 100 mL volumetric flask, and carrying out constant volume to a scale by using acetonitrile to obtain a secondary standard stock solution. Standard stock solutions were stored protected from light, -18 ℃. Transferring secondary standard stock solutions with different volumes, diluting the secondary standard stock solutions with blank sample extracting solutions, and finally preparing standard working solutions with concentration gradients;
the method comprises the following steps: the secondary standard stock solution was transferred into 6 10 mL volumetric flasks at 25. mu.L, 50. mu.L, 100. mu.L, 250. mu.L, 500. mu.L and 1000. mu.L, respectively, and the volume was determined by using the blank sample extract.
c. Liquid chromatography-mass spectrometry, namely sucking the prepared standard working solutions with different concentrations and injecting the working solutions into a liquid chromatography-mass spectrometer;
d. calculation of measurement result of amount of residual agricultural chemical
Performing quantitative analysis of residual amount by external standard method, i.e. performing regression analysis on corresponding concentration by chromatographic peak area of iprodione metabolite to obtain standard curve with correlation coefficient greater than or equal to 0.99, measuring the chromatographic peak area of the extracted sample to obtain target substance, substituting into the standard curve to obtain residual amount of iprodione metabolite in the sample, and calculating the residual amount of iprodione metabolite in accordance with formula
And calculating to obtain the content of iprodione in the sample.
The liquid chromatography conditions used were: a chromatographic column: atlantis T3 (150 mm. times.2.1 mm, 3.0 μm); mobile phase A: acetonitrile; mobile phase B0.1% formic acid solution in water (volume fraction); isocratic elution, mobile phase a: mobile phase B =4: 1; flow rate: 0.2 mL/min; column temperature: 40 ℃; sample introduction amount: 10 mu L of the solution; the mass spectrometry conditions used were: the scanning mode is as follows: negative ion scanning, electrospray ion source (ESI), atomizing gas flow rate of 60 psi, gas curtain gas flow rate of 20 psi, auxiliary heating gas flow rate of 60 psi, ionization temperature of 500 ℃, residence time of 100 msec, ionization voltage of 5500V, and Q1 scanning mode acquisition, wherein the scanning parameters are shown in Table 1.
TABLE 1 monitoring ion and declustering Voltage
| Name of Chinese | Quantitative ion | Qualitative ion | Declustering voltage (V) |
| Iprodione metabolites | 243 | 159.9 | -80 |
The method overcomes the defects of the sample treatment method in the prior art, and optimizes the sample pretreatment method and the instrument detection conditions aiming at the characteristics of iprodione and metabolites thereof. Compared with the prior art, the method has the following excellent effects:
(1) since the iprodione in the sample is easy to decompose to generate the iprodione de- (N-isopropyl formamide), the residual condition of the iprodione in the sample cannot be accurately evaluated only by detecting the content of the iprodione in the sample. According to the invention, the iprodione in the sample is completely converted into the iprodione de- (N-isopropyl formamide) in an alkaline environment, the total amount of the iprodione in the sample is indirectly determined by determining the content of the iprodione de- (N-isopropyl formamide), the experimental operation is simple and rapid, and the blank of the determination of the substances is filled.
(2) The method has the advantages of accurate operation, high sensitivity and good repeatability.
Detection limit of the method of the invention:
the standard working solutions of different concentrations were injected into LC-MS and the limit of detection (LOD) was calculated as 3 times the signal-to-noise ratio (S/N = 3), with a limit of detection of 0.08 mg/kg.
The repeatability and the standard recovery rate of the method are as follows:
a standard solution of iprodione metabolite was added to a blank tobacco sample, and then a pretreatment and LC-MS analysis were performed, and the recovery rate was calculated according to the addition amount and the measured value, and the results are shown in Table 2. As can be seen from Table 2, the average recovery rate of the iprodione metabolite was 90.8%, and the average Relative Standard Deviation (RSD) was less than 5%, indicating that the method of the present invention has high recovery rate and good reproducibility.
TABLE 2 recovery and repeatability (n = 5)
Drawings
FIG. 1 is a flow chart of the measurement method of the present invention (the figure is an abstract figure).
FIG. 2 is a selective ion chromatogram of a spiked sample according to the present invention.
Detailed Description
The invention is further described below with reference to examples, but without limiting the invention.
Example 1:
1. instruments and reagents:
the pesticides are all standard products; acetonitrile and formic acid are both pesticide residue grades.
An API 4000 quadrupole tandem mass spectrometer; vortex oscillator (Labnet corporation, usa); sigma 3-30K centrifuge (Sigma, Germany); AE 163 electronic balance (inductance: 0.0001 g) and AE 166 electronic balance (inductance: 0.01 g) (Mettler, Switzerland).
2. Sample treatment:
accurately weigh 1.0 g of sample (to the nearest 0.01 g) into a 50 mL centrifuge tube with a lid. 18 mL of 0.2 moL/L sodium hydroxide solution was added, and the tube was placed on a vortex mixer shaker and shaken at 2000 rpm for 2 min. Then placing in a water bath kettle at 90 deg.C for 30 min. Cooling to room temperature, adding 2.0 mL of hydrochloric acid solution with the mass fraction of 30%, mixing uniformly, adding 10 mL of dichloromethane, and oscillating at the speed of 2000 rpm for 2 min. Sucking 1mL of lower layer clear liquid, blowing nitrogen to be nearly dry, re-dissolving with 1.0 mL of acetonitrile, filtering by a 0.45-micron organic phase filter membrane, and detecting by LC-MS;
3. preparation of standard working solutions: respectively weighing 10 mg (accurate to 0.1 mg) of iprodione metabolite standard substance in a 10 mL volumetric flask, selecting acetonitrile to dissolve according to the solubility of the standard substance, and fixing the volume to scale to prepare a first-level standard stock solution. And transferring 1.0 mL of standard stock solution into a 100 mL volumetric flask, and carrying out constant volume to a scale by using acetonitrile to obtain a secondary standard stock solution. Standard stock solutions were stored protected from light, -18 ℃. The secondary standard stock solutions were transferred to 6 10 mL volumetric flasks at 25. mu.L, 50. mu.L, 100. mu.L, 250. mu.L, 500. mu.L and 1000. mu.L, respectively, and the volume was determined with acetonitrile.
4. The determination method comprises the steps of injecting prepared standard working solutions with different concentrations into LC-MS, and carrying out quantitative analysis on the residual quantity by an external standard method, namely carrying out regression analysis on the corresponding concentrations of the iprodione metabolites by using the chromatographic peak areas of the iprodione metabolites to obtain a standard curve, wherein the correlation coefficient is more than or equal to 0.99. And (4) measuring the extracted sample, measuring the chromatographic peak area of the iprodione metabolite, substituting the chromatographic peak area into a standard curve, and obtaining the residual amount of the iprodione metabolite in the sample. The content of iprodione metabolites in the samples was found to be 0.32 mg/kg, respectively, and the content of iprodione calculated to be 0.43 mg/kg.
The liquid chromatography conditions used were: a chromatographic column: atlantis T3 (150 mm. times.2.1 mm, 3.0 μm); mobile phase A: 0.1% formic acid acetonitrile solution (volume fraction); mobile phase B0.1% formic acid solution in water (volume fraction); isocratic elution, mobile phase a: mobile phase B =4: 1; flow rate: 0.2 mL/min; column temperature: 40 ℃; sample introduction amount: 10 mu L of the solution; the mass spectrometry conditions used were: the scanning mode is as follows: negative ion scanning, electrospray ion source (ESI), atomizing gas flow rate of 60 psi, gas curtain gas flow rate of 20 psi, auxiliary heating gas flow rate of 60 psi, ionization temperature of 500 ℃, residence time of 100 msec, ionization voltage of 5500V, and Q1 scanning mode acquisition.
For judging the accuracy of the method, the sample is added with the standard solution to ensure that the theoretical content of the iprodione metabolite in the sample is 0.50 mg/kg, the sample pretreatment is carried out as above, the quantitative ion peak area of the iprodione metabolite is measured by LC-MS and is substituted into a standard curve to obtain that the content of the iprodione metabolite in the sample is 0.48 mg/kg, and the addition recovery rate is 88.9%.
Example 2:
another tobacco sample was selected as described in example 1, and the iprodione metabolite [ iprodione de- (N-isopropyl formamide) ] was not detected in the sample.
Claims (3)
1. A high performance liquid chromatography-mass spectrometry method for iprodione in tobacco and tobacco products is characterized in that: decomposing all the iprodione in the sample into metabolites, namely iprodione de- (N-isopropyl formamide), acidifying by hydrochloric acid, performing liquid-liquid extraction by using dichloromethane, filtering, blowing nitrogen to be nearly dry, re-dissolving by using acetonitrile, and measuring the content of the iprodione metabolites in the sample by using liquid chromatography-mass spectrometry so as to indirectly measure the content of the iprodione in the sample;
the liquid chromatography conditions used were: a chromatographic column: atlantis T3, specification 150 mm × 2.1mm, 3.0 μm; mobile phase A: 0.1% formic acid acetonitrile solution; mobile phase B is 0.1% formic acid water solution; isocratic elution, mobile phase a: mobile phase B =4: 1; flow rate: 0.2 mL/min; column temperature: 40 ℃; sample introduction amount: 10 mu L of the solution; the mass spectrometry conditions used were: the scanning mode is as follows: electrospray ion source (ESI); the atomized air flow is 60 psi, and the air curtain flow is 20 psi; the auxiliary heating air flow rate was 60 psi; the ionization temperature is 500 ℃; the stay time is 100 msec; ionization voltage 5500V, Q1 scan mode acquisition.
2. The method for measuring high performance liquid chromatography-mass spectrometry of iprodione in tobacco and tobacco products according to claim 1, wherein: the determination method comprises the following specific steps:
a. and (3) extracting a sample: accurately weighing 1.0 g of sample into a 50 mL centrifuge tube with a cover, adding 18 mL of 0.2 moL/L sodium hydroxide solution, then placing the centrifuge tube on a vortex mixing and oscillating instrument, oscillating for 2 min at the speed of 2000 rpm, then placing the centrifuge tube in a water bath kettle at 90 ℃ for 30min, cooling to room temperature, adding 2.0 mL of hydrochloric acid solution with the mass fraction of 30%, uniformly mixing, then adding 10 mL of dichloromethane, oscillating for 2 min at the speed of 2000 rpm, sucking 1mL of lower clear liquid, blowing nitrogen to be dry, redissolving with 1.0 mL of acetonitrile, filtering through a 0.45 mu m organic phase filter membrane, and detecting by LC-MS;
b. preparation of standard working solution: weighing 10 mg of iprodione metabolite standard substance in a 10 mL volumetric flask, selecting acetonitrile according to the solubility of the standard substance for dissolving, and fixing the volume to a scale to prepare a primary standard stock solution; transferring 1.0 mL of standard stock solution into a 100 mL volumetric flask, and carrying out constant volume to a scale by using acetonitrile to obtain a secondary standard stock solution; storing the standard stock solution at-18 ℃ in a dark place; transferring secondary standard stock solutions with different volumes, diluting the secondary standard stock solutions with blank sample extracting solutions, and finally preparing standard working solutions with concentration gradients;
c. liquid chromatography-mass spectrometry, namely sucking the prepared standard working solutions with different concentrations and injecting the working solutions into a liquid chromatography-mass spectrometer;
d. calculation of the pesticide residue amount measurement result:
performing quantitative analysis of residual amount by external standard method, i.e. performing regression analysis on corresponding concentration by chromatographic peak area of iprodione metabolite to obtain standard curve with correlation coefficient greater than or equal to 0.99, measuring the chromatographic peak area of the extracted sample to obtain target substance, substituting into the standard curve to obtain residual amount of iprodione metabolite in the sample, and calculating the residual amount of iprodione metabolite in accordance with formula
And calculating to obtain the content of iprodione.
3. The method for measuring high performance liquid chromatography-mass spectrometry of iprodione in tobacco and tobacco products according to claim 2, wherein: the standard working solution with concentration gradient finally prepared in the step b is prepared in the following way: the secondary standard stock solution was transferred into 6 10 mL volumetric flasks at 25. mu.L, 50. mu.L, 100. mu.L, 250. mu.L, 500. mu.L and 1000. mu.L, respectively, and the volume was determined by using the blank sample extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811429923.3A CN109212109B (en) | 2018-11-28 | 2018-11-28 | High performance liquid chromatography-mass spectrometry determination method for iprodione in tobacco and tobacco products |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811429923.3A CN109212109B (en) | 2018-11-28 | 2018-11-28 | High performance liquid chromatography-mass spectrometry determination method for iprodione in tobacco and tobacco products |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109212109A CN109212109A (en) | 2019-01-15 |
| CN109212109B true CN109212109B (en) | 2021-01-26 |
Family
ID=64993958
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811429923.3A Active CN109212109B (en) | 2018-11-28 | 2018-11-28 | High performance liquid chromatography-mass spectrometry determination method for iprodione in tobacco and tobacco products |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109212109B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112684034A (en) * | 2020-12-10 | 2021-04-20 | 中国烟草总公司郑州烟草研究院 | Non-target analysis method for detecting tobacco and tobacco products based on HPLC-QTOF MS technology |
| CN112684033A (en) * | 2020-12-10 | 2021-04-20 | 中国烟草总公司郑州烟草研究院 | High performance liquid chromatography-quadrupole time-of-flight mass spectrometry detection method for buccal tobacco non-targeted analysis |
| CN113295801B (en) * | 2021-06-04 | 2023-04-25 | 国家烟草质量监督检验中心 | Method for determining fipronil in plant-derived food |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106324123A (en) * | 2016-08-09 | 2017-01-11 | 国家烟草质量监督检验中心 | Determination method of pesticide residual quantity in tobacco and tobacco products |
| CN106970169A (en) * | 2017-05-08 | 2017-07-21 | 新疆维吾尔自治区分析测试研究院 | The method that liquid chromatography tandem mass spectrometry determines antiseptic and fresh-keeping agent for fruits residual quantity |
-
2018
- 2018-11-28 CN CN201811429923.3A patent/CN109212109B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106324123A (en) * | 2016-08-09 | 2017-01-11 | 国家烟草质量监督检验中心 | Determination method of pesticide residual quantity in tobacco and tobacco products |
| CN106970169A (en) * | 2017-05-08 | 2017-07-21 | 新疆维吾尔自治区分析测试研究院 | The method that liquid chromatography tandem mass spectrometry determines antiseptic and fresh-keeping agent for fruits residual quantity |
Non-Patent Citations (3)
| Title |
|---|
| Residual Pattern and Dietary Intake of Iprodione on Grapes under Egyptian Field Conditions: A Prelude to Risk Assessment Profile;Naglaa Loutfy et al.;《Human and Ecological Risk Assessment》;20140825;第265-279页 * |
| 固相萃取-液相色谱分析蔬菜中噻菌灵和苯菌灵残留量;吴刚 等;《检验检疫科学》;20081231;第24-26页 * |
| 异菌脲在苹果及土壤中残留量的测定方法;宋国春 等;《农药科学与管理》;20041231;第10-12页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109212109A (en) | 2019-01-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109212109B (en) | High performance liquid chromatography-mass spectrometry determination method for iprodione in tobacco and tobacco products | |
| CN106053703B (en) | It is a kind of at the same detect food in various plants growth regulator method | |
| CN104614466B (en) | The assay method of antiseptic in tobacco juice for electronic smoke | |
| CN102854271A (en) | Method for measuring residues of three phenoxy carboxylic acid pesticides in tobacco and tobacco products | |
| CN108760672A (en) | The detection method of melamine | |
| CN102944636B (en) | High-efficiency liquid chromatography to mass spectrum detection method for ethyl carbamate in distilled liquor | |
| CN111351872B (en) | HPLC (high performance liquid chromatography) detection method for residual quantity of sincalide in food | |
| CN108020627B (en) | Method for determining residual quantity of three phenoxy carboxylic acid pesticides in tobacco by ultra-high performance synthetic phase chromatography-tandem mass spectrometry | |
| CN103123345B (en) | Method for rapidly detecting phenoxyacetic acid herbicide in soil | |
| CN107688062A (en) | A kind of method of trace nicotine in measure tobacco juice for electronic smoke | |
| CN108760920B (en) | Method for determining residual quantity of cyazofamid and metabolites thereof based on HPLC-MSMS method | |
| CN107037151B (en) | A kind of measuring method of transfer volume of epoxy chloropropane in food contact material | |
| CN109507354B (en) | Method for determining content of K powder in human hair by flash evaporation-gas chromatography-mass spectrometry | |
| CN108181394A (en) | The method that a kind of extraction-purification Synchronos method measures three kinds of phenoxy carboxylic acid persticide residues in tobacco | |
| Jiang et al. | Rapid determination of dimethoate in nanoliter of juice using surface desorption atmospheric pressure chemical ionization mass spectrometry | |
| Wang et al. | A comprehensive strategy for screening and exploring multi-class mycotoxins contamination status in Astragali Radix | |
| CN110082450A (en) | It is a kind of weight-reducing class Chinese patent drug and health food in piperine detection method | |
| CN109212076B (en) | Method for detecting oxyfluorfen in water by using HPLC-MS/MS method | |
| CN109239241A (en) | The measuring method of my acid benzene-S-methyl in a kind of tobacco and tobacco product | |
| CN107831228B (en) | Method and kit for determining citronellal in sample and application of kit | |
| CN115032312B (en) | Method for simultaneously detecting multiple sensitization fragrances in mosquito-repellent product | |
| CN109633071B (en) | Method for detecting Saisentong copper in water by using UPLC-MS/MS method | |
| CN113588844B (en) | High-sensitivity detection method for glycol substances in aqueous food simulant | |
| CN113341039B (en) | Sample pretreatment method and determination method for determining coumoxystrobin and/or pyraclostrobin in plant-derived food | |
| CN109738566B (en) | Method for detecting oxine-copper in water by using UPLC-MS/MS method |
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 |