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GB 29382-2012: Mesotrione technical material
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GB 29382-2012: Mesotrione technical material

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Mesotrione technical material ICS 65.100.20 G25 National Standards of People's Republic of China Mesotrione TC Published 2012-12-31 2013-07-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China issued

Foreword

This standard in Chapter 3, Section 5 is mandatory, the rest are recommended. This standard was drafted in accordance with rules GB/T 1.1-2009 given. Please note that some of the content of this document may involve patents, the issuing authority of this document does not assume responsibility for identifying these patents. The standard proposed by China Petroleum and Chemical Industry Federation. This standard by the National Pesticide Standardization Technical Committee (SAC/TC133). This standard is drafted. Shenyang Chemical Research Institute Co., Ltd. Participated in the drafting of this standard. Shenyang Branch Chemical Co., Ltd. Limin Chemical Co., Ltd., Jiangsu Changqing Agrochemical Co. shares The company, Shijiazhuang City, three rural Chemical Co., Ltd., Jiangsu Ampang Electrochemical Co., Ltd.. The main drafters. Hou Chunqing, Zhang Xuebing, Li Dong, CHENG Chun, Zhang Ruifang, Ji Yuping, Xie Yueqing, Jiang Yutian, Tao Chengbin. Mesotrione TC

1 Scope

This standard specifies the mesotrione original drug of requirements, test methods and marking, labeling, packaging, storage, and acceptance period. This standard applies to impurities derived from mesotrione composition and production of the original drug mesotrione. NOTE. mesotrione and other names, structural formulas and physicochemical parameters related impurities nitro substantially xanthone see Appendix A.

2 Normative references

The following documents for the application of this document is essential. For dated references, only applies to the version dated paper Pieces. For undated references, the latest edition (including any amendments) applies to this document. Determination 1601 pH value pesticides GB/T GB/T 1604 pesticide regulations for acceptance of goods GB/T 1605-2001 sampling commercial pesticides GB 3796 pesticide packaging General GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD) GB/T 8170-2008 rounding off means about rules and determining limiting values GB/T 19138 Determination of acetone insoluble pesticide 3.1 Appearance As a light brown to yellow-brown solid powder, or wet brown solid, without visible foreign matter and added modifier. 3.2 Technical Specifications Mesotrione TC shall comply with the requirements in Table 1. Table 1 TC mesotrione control program Index Item Index Mesotrione mass fraction (dry basis) /% ≥ 95.0 Loss on drying /% ≤ 25 Xanthone, thioxanthone nitro mass fraction a (dry basis)/(mg/kg) ≤ 2 Acetone insolubles a /% ≤ 0.2 The pH range of 3.0 to 6.0 When a normal production, nitro xanthone mass fraction insoluble in acetone was measured at least once every three months. Test Method 4 Safety Tips. to use this standard shall have practical experience of laboratory work. This standard does not indicate any safety issues. Make With those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the provisions of relevant state laws and regulations. 4.1 General provisions This standard reagent in the absence of water and other requirements stated, refer to three predetermined analytical reagents and GB/T 6682-2008 of water. The test results performed by determining 4.3.3 rounding value in comparison 8170-2008 GB/T . 4.2 Sampling Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determining Sample packages with a random number table method; final sample size Not less than 100g. 4.3 Identification Test Infrared spectroscopy --- mesotrione sample and standard ~ 400cm-1 in the infrared range of 1 4000cm-absorption spectrum should not expressly Significant difference. Mesotrione standard infrared spectra of Figure 1. FIG 1 mesotrione standard infrared spectrum of FIG. The present liquid chromatography --- identification test can be conducted simultaneously with the determination of one mass fraction sulcotrione nitrate. Chromatography under the same operating conditions, Main peaks of the sample solution and the retention time of the solution of the mesotrione sample peak retention time scale, the relative difference of 1.5% should be Or less. Determination of mass sulcotrione nitro ketone score 4.4 4.4.1 Method summary After drying in vacuo a sample was dissolved in mobile phase, acetonitrile and water (phosphate adjusted to pH 3) as the mobile phase, used as a filler C18 Stainless steel column and a UV detector at a wavelength of 270nm, the sample of mesotrione reverse phase high performance liquid chromatography and determination, External standard. 4.4.2 Reagents and solutions Acetonitrile. HPLC grade; Water. The new secondary steam distilled water; Phosphoric acid; Mesotrione Sample. a known mass fraction, w≥99.0%. 4.4.3 Instruments HPLC. a variable wavelength UV detector; Chromatographic data processor or chromatography workstation; Column. 250mm × 4.6mm (id) stainless steel column, C18,5μm filler contents (or column with equivalent effect); Filter. membrane pore size of about 0.45 m; Microsyringe. 50μL; Quantitative sampling tube. 5μL; Ultrasonic cleaning. 4.4.4 HPLC operating conditions Mobile phase. [Psi] [acetonitrile. water (adjusted to pH 3 phosphate to)] = 40.60, by membrane filtration, and degassing; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should be less than 2 deg.] C); Detection wavelength. 270nm; Injection Volume. 5μL; Retention time. mesotrione about 10.1min. Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result. Typical mesotrione HPLC TC shown in Figure 2. 1 --- mesotrione. Figure 2 HPLC mesotrione original drug 4.4.5 Determination Step 4.4.5.1 Preparation of standard solution 0.1 g of weighed (accurate to 0.0002g) mesotrione standard in 50mL volumetric flask, dilute to the mark with acetonitrile, ultrasonic oscillation 5min to dissolve the sample, cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, dilute with the mobile phase Release to the mark. 4.4.5.2 Preparation of sample solution Weigh mesotrione containing 0.1 g of (accurate to 0.0002g) sample had been dried (drying method of section 4.5.2) in a 50mL volumetric flask , Washed with acetonitrile to volume, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaking. Pipette with a pipette to the solution 5mL, 50mL volumetric flask, diluted in phase with the flow to the mark. 4.4.5.3 Determination Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two adjacent needles mesotrione peak area becomes relatively After of less than 1.5%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution. 4.4.5.4 computing The two needle and the sample solution was measured before and after the sample solution two needle mesotrione standard peak area are averaged. Mesotrione sample Oxadiazon mass fraction according to formula (1). w1 = A2 · M1 · w A1 · m2 (1) Where. W1 --- mesotrione sample mass fraction in%; A2 --- sample solution, nitro sulcotrione one average peak area; M1 --- mesotrione standard mass in grams (G); W --- the mass fraction mesotrione standard sample, expressed in%; A1 --- the standard solution, mesotrione average peak area; --- M2 sample mass, in grams (g). 4.4.6 allows poor Ketone mass difference mesotrione Results replicates grass two fractions should be not more than 1.5%, and the arithmetic mean value as a measurement result. 4.5 Determination of loss on drying 4.5.1 Instruments Vacuum pump; Vacuum oven. 60 ℃ ± 2 ℃, exemplar vacuum pressure. -90kPa ± 5kPa. 4.5.2 Determination Step Weigh 10g weighing bottle with the sample constant weight (accurate to 0.01g), paving, placed in a vacuum oven. Vacuum pump was turned on 60 ℃ ± 2 ℃, exemplar vacuum dried to constant weight (about 1h) -90kPa ± 5kPa depressed condition in a desiccator, cooled to room temperature, Weighed. 4.5.3 computing Loss on drying the sample by the formula (2). w2 = m0-m1m × 100 (2) Where. --- w2 of the sample mass fraction of drying loss, expressed in%; Mass M0 --- weighing bottle and the sample in grams (G); Mass M1 --- dried weighing bottle and the sample in grams (G); --- m sample mass, in grams (g). Determination of the mass fraction of 4.6 nitro thioxanthone xanthone 4.6.1 Method summary Sample was dissolved in acetonitrile, using a liquid chromatography tandem quadrupole mass spectrometer, using MRM mode, the sample nitro xanthones Tandem mass spectrometry for detection, based on the extracted ion chromatogram obtained external standard. 4.6.2 Reagents and solutions Acetonitrile. HPLC grade; Water. The new secondary steam distilled water; Ammonium acetate; Ammonium acetate solution [c (CH3COONH4) = 5mmol/L]. 0.375g weighed (accurate to 0.0002g) ammonium acetate in a 1L capacity Volumetric flask, dilute to the mark with water, shake, filter; Mesotrione sample. no nitro xanthone; Nitro xanthone Sample. a known mass fraction, w≥90.0%. 4.6.3 Instruments Liquid chromatography - tandem quadrupole mass spectrometer; Column. 150mm × 4.6mm (id) stainless steel column, C18,5μm filler contents (or column with equivalent effect); Filter. membrane pore size of about 0.22 m; Autosampler. 5μL; Ultrasonic cleaning. 4.6.4 HPLC operating conditions Mobile phase. [Psi] (acetonitrile. ammonium acetate solution) = 50.50, by membrane filtration, and degassing; Flow rate. 0.5mL/min, 5.5min ~ 10min into the mass; Column temperature. 40 ℃; Injection Volume. 5μL; Retention time. nitro xanthone about 7.2min. 4.6.5 Mass operating conditions Ion source. APCI (-); Source temperature. 130 ℃; Desolvation temperature. 550 ℃; Cone voltage. 20V; Collision gas. argon; Collision energy. 30V; Scan mode. MRM, parent ion 344; 207 ions; The above are typical operating parameters, depending on the instrument type may, for a given operating parameters appropriately adjusted to obtain the best result. Typical mesotrione TC extracted ion chromatograms shown in Figure 3. 1 --- nitro xanthone. LC extracted ion chromatograms of FIG. 3 mesotrione TC nitro xanthone 4.6.6 Determination Step 4.6.6.1 Preparation of working standard Preparation of standard solution. Weigh 0.01g (accurate to 0.0002g) xanthone-nitro-Standard in 100mL volumetric flask to volume with acetonitrile To the mark to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shake (solution 1). Pipette solution 1mL to 10mL pipetted Volumetric flask, dilute to the mark with acetonitrile, shake (solution 2). Then pipette 5mL aliquot solution in 50mL volumetric flask with acetonitrile Dilute to volume, mix (solution 3). Weigh 0.5g (accurate to 0.0002g) containing no nitro xanthone mesotrione sample in 10mL stoppered vial, added with a pipette 3 into 5mL solution, to dissolve the sample ultrasonic vibration 5min, cooled to room temperature, shaken and filtered to give standard solution. 4.6.6.2 Preparation of sample solution Weigh 0.5g (accurate to 0.0002g) mesotrione sample in 10mL stoppered vials, with a pipette 5mL of acetonitrile was added, over To dissolve the sample acoustic shock 5min, cooled to room temperature, shaken and filtered. 4.6.6.3 Determination Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the extracted ion chromatogram two adjacent needles nitro xanthene Thioxanthone peak area relative changes of less than 30%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution. 4.6.6.4 computing The two needle and the sample solution was measured before and after the two doses of the standard sample solution nitro xanthone peak area are averaged. Sample Xanthone content nitro peaks by formula (3) is calculated. w3 = A2 · M1 · w 2000A1 · m2 × 106 (3) Where. --- the mass fraction of the sample W3 nitro xanthone peaks to in mg/kg; A2 --- sample solution, nitro xanthone average peak area; M1 --- nitro xanthone standard mass in grams (G); W --- the mass fraction nitro xanthone standard sample, expressed in%; --- 2000 dilution; A1 --- the standard solution, nitro xanthone average peak area; --- M2 sample mass, in grams (g). 4.6.7 allows poor Nitro ketone mass xanthene parallel relative deviation measurement result two fractions should be not more than 30%, and the arithmetic mean value as a measurement result. 4.7 pH value measured Carried out in GB/T 1601. 4.8 Determination of acetone insolubles 5g weighed (accurate to 0.01g) sample, according to GB/T 19138 Determination of acetone insolubles. 4.9 product testing and acceptance Shall comply with the provisions of GB/T 1604's. 5 marking, labeling, packaging, storage, security and acceptance of 5.1 marking, labeling, packaging Flag mesotrione original drug, labeling and packaging should comply with the provisions of GB 3796. Mesotrione original medicinal lined metal containers loaded barrel net Content is generally 50kg or 100kg. The original amount of drug loaded barrel should not exceed 1/2 of volume, according to user requests or orders RA Discuss other forms of packaging, subject to the provisions of GB 3796, the original dose per barrel loaded should not exceed 1/2 of volume. 5.2 Storage Mesotrione original drug package airiness, dry place. Storage and transportation, prevent moisture and sunlight, storage temperature should be no higher than 45 ℃, not mix with food, seed, feed, to avoid contact with the skin, eyes, mouth and nose to prevent inhalation. 5.3 Security This product is of low toxicity herbicide. Should wear rubber gloves and goggles necessary to wear protective clothing while the FDA. After spraying with soap and Rinse with water. Coverage should be immediately sent to hospital for symptomatic treatment. 5.4 Acceptance of Acceptance of mesotrione original drug for 1 month. From the date of delivery, product quality inspection completed within a month, its targets were It should meet the standards.

Appendix A

(Informative) Mesotrione names and other related impurities nitro xanthone, and the basic physicochemical parameters of the formula This product is an active ingredient of other names, formulas and basic physicochemical parameters of mesotrione is as follows. ISO common name. mesotrione CAS Registry Number. 104206-82-8 Chemical Name. 2- (4-methanesulfonyl-2-nitrobenzoyl) cyclohexane-1,3-dione Structure. Empirical formula. C14H13NO7S Molecular weight. 339.3 Biological activity. weeding Melting point. 148.7 ℃ ~ 152.5 ℃ Solubility (20 ℃). water 0.16mg/L; xylene 1.4g/L, toluene, 2.7g/L, methanol 3.6g/L, acetone 76.4g/L, methylene chloride 82.7g/L, acetonitrile 96.1g/L. Stability. stable water pH5 ~ 9, the original drug reservoir 14d is stable at 54 ℃. Nitro impurities in the product name xanthone, structural formulas and physicochemical basic parameters are as follows. Common name. Nitro xanthone Chemical Name. 1-cyano-6- (methylsulfonyl) -7-nitro -9H- xanthene-9-one Structure. Empirical formula. C15H8N2O6S Molecular weight. 344.0 Solubility. acetonitrile 10mg/100mL; dimethylsulfoxide > 1mg/mL Stability. decomposition above 120 deg.] C. 2102- ...