Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2217-91
Atrazine Wettable Powder
Published on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1992
Chemical Industry Standard of the People's Republic of China
Atrazine Wettable Powder
HG 221791Www.bzxZ.net
This standard adopts the United Nations Food and Agriculture Organization (UNFAO) standard FAO91/3/S/7 "Atrazine Wettable Powder" subject content and scope of application
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage requirements of 48% Atrazine Wettable Powder.
This standard applies to Atrazine Wettable Powder processed from Atrazine technical material, fillers and adjuvants. Active ingredient: HuCIN
Chemical name: 2-chloro-4-ethylamino-6-isopropylamino-1,3,5-triazine Structural formula:
(CHs),CHNH
Molecular formula: C.HuCIN
NH -C2Hs
Relative molecular mass: 215.69 (according to the international relative atomic mass in 1987) 2 Reference standards
1 Method for determination of hydrogen ion concentration of pesticides
GB1601
GB1605
GB3796
Sampling method for commercial pesticides
General rules for pesticide packaging
GB5451 Method for determination of wettability of pesticide wettable powders HG2-896 Technical requirements for determination of fineness of pesticide powders
3.1 Appearance: Powder without visible foreign matter and lumps. 3.2 The wettable powder of lingzhina should also meet the following technical requirements: Item
lingzhina content, %(m/m)
suspension rate, %(m/m)
wetting time, s
fineness [through 45um (325 mesh) sieve], %(m/m)heat storage stability\
Note, 1) is the type inspection item.
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991AV
48.0±:8
Implemented on July 1, 1992
4 Test method
4.1 Determination of the content of quinazolin (arbitration method) 4.1.1 Summary of the method
HG2217-91
The sample was dissolved in chloroform, and quinazolin was separated and determined on a chromatographic column filled with triadimefon as the internal standard and 3% polyethylene glycol 20000/GasChromQ as the filling material. 4.1.2 Reagents and solutions
Chloroform (GB682);
Polyethylene glycol 20000: Gas Chromatography stationary liquid GasChromQ: 150~180μm (80~100 mesh), carrier for gas chromatography; Internal standard solution: 20g/L triadimefon chloroform solution; Aminotriptyline standard: known content, ≥99% (m/m); Triadimefon: content greater than 95% (m/m), no interferences after gas chromatography analysis. 4.1.3 Instruments
Gas chromatograph: with flame ionization detector; Chromatographic column: stainless steel column with a length of 1.8~2.0m and an inner diameter of 4mm; Carrier: nitrogen, nitrogen content greater than 99.99%, try to filter out oxygen and water; Micro-injector: 10uL.
4.1.4 Determination steps
4.1.4.1 Preparation of chromatographic column
4.1.4.1.1 Coating of stationary liquid
Weigh 0.45g of polyethylene glycol 20000 in a 100mL beaker, add about 45mL of chloroform (just enough to immerse the carrier), and stir to completely dissolve it. Weigh 15.0g of the carrier and pour it into the above beaker at once. Place the beaker in a water bath at about 60℃, and gently shake the beaker from time to time to mix it evenly. When the solvent evaporates to near dryness, place the beaker in a 100℃ oven and dry it for 1h. 4.1.4.1.2 Filling of chromatographic column
Connect a small funnel to the inlet end of the cleaned and dried chromatographic column, and wrap the outlet end with gauze and connect it to the vacuum pump. Turn on the vacuum pump, pour the column filling material from the funnel, and tap the column wall continuously until the filling material stops falling. Remove the chromatographic column and plug a little glass wool at both ends of the column. 4.1.4.1.3 Aging of the chromatographic column
Connect the inlet end of the chromatographic column to the vaporizer, and do not connect the outlet end to the detector. The carrier gas flow rate is 20mL/min. The column temperature is increased from 100℃ to 210℃ in six times within 6h, and aged at this temperature for at least 24h. 4.1.4.2 Chromatographic operating conditions
Temperature:
200±5℃;
Column chamber 2
Vaporizer chamber 230℃;
Detector 230℃.
Gas flow rate:
Carrier gas (N,) 80mL/min;
Hydrogen 40mL/min,
Air 400mL/min.
Injection volume:
Retention time:
Torazine 11min;
Triadimefon: 17min.
HG2217-91
The above chromatographic operating conditions are typical operating parameters. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect. 2
Gas chromatogram of torazine
1-Torazine; 2-Triadimefon
4.1.4.3 Preparation of standard solution and sample solution Weigh the standard and sample containing 0.10g of torazine (accurate to 0.0001g). Place them in stoppered vials respectively, and use a pipette to transfer 5.0mL of internal standard solution into each vial. Shake the vials thoroughly and let them stand. Take the supernatant for injection and filter or centrifuge if necessary. 4.1.4.4 Determination
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the standard solution of chloramphenicol until the relative deviation of the peak height ratio (or peak area ratio) of chloramphenicol to triadimefon between two consecutive injections is less than 0.7%, and then inject in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
4.1.4.5 Calculation
Based on the chromatograms of the four injections a, b, c, and d, calculate the average values of the peak height ratio (or peak area ratio) of chloramphenicol to triadimefon in a, d and b, c, respectively.
The mass percentage of tarazine 1 is calculated according to formula (1): 3
HG2217-—91
12·mi
Wherein: 1——the average value of the peak height ratio (or peak area ratio) of tarazine to triadimefon in the sample solution injected twice in b and c; i2——the average value of the peak height ratio (or peak area ratio) of tarazine to triadimefon in the standard solution injected twice in a and d; the mass of a sample, 8;
m2——the mass of the standard sample, g;
the purity of the standard sample, % (m/m).
4.1.5 Allowable difference
The difference between the results of two parallel determinations in this method shall not exceed 1.0%. 4.2 Determination of suspension rate
4.2.1 Method summary
Weigh 1g of sample and prepare a suspension in a measuring cylinder with standard hard water. Under specified conditions, determine the mass of 1/10 suspension and precipitate at the bottom and calculate its suspension rate. 4.2.2 Solution
Standard hard water: 342ppm. Prepare according to the method in GB5451. 4.2.3 Instrument
Constant temperature water bath: 30±1℃;
Measuring cylinder: with ground stopper, 250mL, the distance between 0~250mL scale line is 20.0~21.5cm, and the distance between 250mL scale line and the bottom of the stopper is 4~6cm;
Glass pipette: about 40cm long, 5mm inner diameter, with a 2~3mm hole at the tip of one end, and the other end connected to the suction source. 4.2.4 Determination steps
Weigh the sample containing 0.5g of moxibustion (accurate to 0.0001g) and slowly put it into a 200mL beaker containing 50mL of standard hard water (30±1℃). Shake the beaker in a circular motion by hand for 2min, 120 times per minute. After the beaker is placed in a 30±1℃ water bath for 13min, transfer the sample quantitatively to a measuring cylinder (about 30℃) with 30±1℃ standard hard water, dilute to 250mL, and plug it. Invert the measuring cylinder upside down 30 times at a speed of once every two seconds. Place the measuring cylinder vertically in a water bath without vibration and direct sunlight for 30min. Then, within 10-15s, use a pipette to draw out 9/10 of the suspension in the upper part of the measuring cylinder. When drawing liquid, the tip of the pipette should be kept a few millimeters below the liquid surface to minimize the agitation of the suspension.
Use a long pipette to suck 1/10 of the residue in the measuring cylinder into a 50mL beaker. Rinse the bottom of the measuring cylinder three times with 15mL of water (avoid washing the sticky material on the top of the measuring cylinder), and transfer it to the beaker. Place the beaker in a 100℃ water bath to evaporate. Weigh 0.23g of chloramphenicol standard sample (accurate to 0.0001g) is placed in a stoppered vial. Use a pipette to transfer 10.0mL of the internal standard solution (4.1.2) to the standard sample vial and the residue beaker, respectively, and determine according to 4.1.4.3 and 4.1.4.4. 4.2.5 Calculation
First calculate the mass of chloramphenicol in 1/10 of the residue according to formula (2), and then calculate the chloramphenicol suspension rate (a2) according to formula (3): mg
m=ms×111.1
Where: ms——the mass of chloramphenicol in 1/10 of the residue, g; m4
——the mass of chloramphenicol in the sample weighed to prepare the suspension, g;——the purity of the standard sample, % (m/m);
111.1——conversion factor.
4.2.6 Allowable difference
The difference between two parallel determination results of this method shall not exceed 5%. 4
…(2)
（3）
4.3 Determination of wetting time
According to GB5451.
4.4 Determination of pH value
According to the pH meter method in GB1601.
4.5 Determination of fineness
According to the wet sieving method in HG2-896.
4.6 Thermal Storage Stability
4.6.1 Apparatus
Beaker: 250mL, inner diameter 6~6.5cm;
HG221791
Metal ball: coated with plastic, diameter slightly smaller than the inner diameter of the beaker, mass to produce a pressure of 2450Pa on its bottom surface; Oven: 54±2℃.
4.6.2 Determination steps
Weigh 20g of sample into a beaker, and spread it into a smooth and uniform layer of equal thickness without using pressure, and place the metal block on the surface of the sample in the beaker. Store the beaker in an oven at 54±2℃ for 14d. Take out the beaker, remove the ball, and put it in a desiccator without desiccant to cool to room temperature. Within 24h, test according to the methods specified in 4.1, 4.3, and 4.5 of this standard. If the results meet the technical requirements of the standard, the thermal storage stability of the product is qualified. 5 Inspection rules
5.1 The quality supervision and inspection department of the production unit shall inspect the humulazine wettable powder. The production unit shall ensure that all the humulazine wettable powders shipped out of the factory meet the requirements of this standard. 5.2 The operating unit and the user unit have the right to inspect whether the received humulazine wettable powder meets the requirements of this standard in accordance with the provisions of this standard.
5.3 The sampling method shall be carried out in accordance with GB1605. The sample shall be divided into two bottles, one bottle shall be sent to the quality supervision and inspection department for inspection, and the other bottle shall be sealed. 5.4 In the inspection results, when there are indicators that do not meet the requirements of this standard, re-sampling shall be conducted from twice the amount of packaging. In the results of the re-inspection, even if one indicator does not meet the requirements of this standard, the entire batch of humulazine wettable powder is an unqualified product. 5.5 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation between the two parties, or the statutory inspection agency can conduct arbitration analysis according to the inspection method specified in this standard.
5.6Under normal circumstances, the inspection cycle of type inspection items shall not exceed one quarter. 6 Marking, packaging, transportation and storage
6.1 Marking and packaging shall comply with the relevant provisions of GB3796. 6.2 During transportation and storage, it shall be strictly protected from moisture and sunlight, and maintained with good ventilation. It shall not be mixed with food, seeds, and feed, and shall avoid contact with the skin to prevent inhalation through the mouth and nose.
6.3 The warranty period of this product is two years. That is, under normal packaging and storage conditions, the content of quinolones shall meet the technical requirements specified in this standard within two years from the date of leaving the factory.
A1 Method Summary
HG2217-91
Appendix A
Gas chromatography determination method for amantadine content
(Supplement)
The sample was dissolved in dimethylformamide, and amantadine was separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS chromatographic column with simethoxazole as the internal standard.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 60g simetholine dimethylformamide solution; Aminotriptyline standard sample: known content, >99% (m/m); simetholine: content ≥95% (m/m), no interferences after gas chromatography analysis; Gas chromatograph: with flame ionization detector; Chromatographic column: 2m long, 4mm inner diameter stainless steel column, filled with 5% XE-60/ChromosorbW/AW-DMCS (150~180um); Micro-injector: 10uL.
Chromatographic operating conditions
Temperature:
Column chamber 212℃;
Vaporization chamber 250℃;
Detector 250℃.
Gas flow rate:
Carrier gas (N)
20mL/min;
Hydrogen 30mL/min;
500mL/min.
Injection volume:
lμL.
Retention time:
Atrazine 7min;
Simethoine 11min.
The above chromatographic operating conditions are typical operating parameters. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect. A4 Preparation of standard solution and sample solution
HG221791
Figure A1 Gas chromatogram of Atrazine
1—Atrazine; 2—Simethoine
Weigh the standard and sample containing 0.08g of atrazine (accurate to 0.0001g) and place them in stoppered vials respectively. Use a pipette to transfer 2.0 mL of internal standard solution into each vial. Shake the vial thoroughly, let it stand, and take the supernatant for sampling. Centrifuge or filter if necessary. A5 Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the sirtuin standard solution until the relative deviation of the peak height ratio of sirtuin to sirtuin in two consecutive injections is less than 0.7%. Then inject in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
A6 Calculation
The mass percentage of squalane (ar) is calculated according to formula (A1): ism..w
In the formula, rs——the average value of the peak height ratio of squalane to squalane in the sample solution injected twice in b and c; rs——the average value of the peak height ratio of squalane to squalane in the standard solution injected twice in a and d; the mass of the sample, 8;
——the mass of the standard sample, g;
w——the purity of the standard sample, % (m/m).
A7 Allowable difference
The difference between the results of two parallel determinations in this method should not exceed 1.0%. (A1)
Additional instructions:
HG2217—91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Wu Qi, Zhang Xuebing, Wang Yufan, Wang Shiyan, Wang Fengfengqin and Zheng Taiyong.2 Determination steps
Weigh 20g of the sample into a beaker and spread it into a smooth and uniform layer of equal thickness without using pressure. Place the metal block on the surface of the sample in the beaker. Store the beaker in an oven at 54±2℃ for 14 days. Take out the beaker, take out the round block, and cool it to room temperature in a desiccator without desiccant. Within 24 hours, test according to the methods specified in Articles 4.1, 4.3, and 4.5 of this standard. If the results meet the technical requirements of the standard, the thermal storage stability of the product is qualified. 5 Inspection rules
5.1 The wettable powder of thiophene should be inspected by the quality supervision and inspection department of the production unit. The production unit shall ensure that all wettable powders of thiophene leaving the factory meet the requirements of this standard. 5.2 The operating unit and the user unit have the right to inspect whether the wettable powder of thiophene received meets the requirements of this standard in accordance with the provisions of this standard.
5.3 The sampling method shall be carried out in accordance with GB1605. The sample should be divided into two bottles, one bottle is sent to the quality supervision and inspection department for inspection, and the other bottle is sealed. 5.4 In the test results, when there are indicators that do not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. In the re-test results, even if one indicator does not meet the requirements of this standard, the entire batch of Motujin wettable powder is an unqualified product. 5.5 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation between the two parties, or the statutory inspection agency can conduct arbitration analysis according to the inspection methods specified in this standard.
5.6 Under normal circumstances, the inspection cycle of type inspection items shall not exceed one quarter. 6 Marking, packaging, transportation and storage
6.1 Marking and packaging shall comply with the relevant provisions of GB3796. 6.2 During transportation and storage, it should be strictly prevented from moisture and sunlight, maintain good ventilation, and shall not be mixed with food, seeds, and feed. Avoid contact with the skin to prevent inhalation through the mouth and nose.
6.3 The warranty period of this product is two years. That is, under normal packaging and storage conditions, the content of quinolones should meet the technical requirements specified in this standard within two years from the date of leaving the factory.
A1 Method Summary
HG2217-91
Appendix A
Gas chromatography determination method for quinolones content
(Supplement)
The sample was dissolved in dimethylformamide, and simethoxazole was used as the internal standard. The quinolones were separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 60g simetholine dimethylformamide solution; Moxifen standard sample: known content, >99% (m/m); simetholine: content ≥95% (m/m), no interferences after gas chromatography analysis; Gas chromatograph: with flame ionization detector; Chromatographic column: 2m long, 4mm inner diameter stainless steel column, filled with 5% XE-60/ChromosorbW/AW-DMCS (150~180um); Micro-injector: 10uL.
Chromatographic operating conditions
Temperature:
Column chamber 212℃;
Vaporization chamber 250℃;
Detector 250℃.
Gas flow rate:
Carrier gas (N)
20mL/min;
Hydrogen 30mL/min;
500mL/min.
Injection volume:
lμL.
Retention time:
7min for atrazine;
11min for simethoprim.
The above chromatographic operating conditions are typical operating parameters. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect. A4 Preparation of standard solution and sample solution
HG221791
Figure A1 Gas chromatogram of atrazine
1—atrazine; 2—simethoprim
Weigh the standard and sample containing 0.08g atrazine (accurate to 0.0001g) and place them in stoppered vials respectively. Use a pipette to transfer 2.0 mL of internal standard solution into each vial. Shake the vial thoroughly, let it stand, and take the supernatant for sampling. Centrifuge or filter if necessary. A5 Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the sirtuin standard solution until the relative deviation of the peak height ratio of sirtuin to sirtuin in two consecutive injections is less than 0.7%. Then inject in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
A6 Calculation
The mass percentage of squalane (ar) is calculated according to formula (A1): ism..w
In the formula, rs is the average value of the peak height ratio of squalane to squalane in the sample solution injected twice in b and c; rs is the average value of the peak height ratio of squalane to squalane in the standard solution injected twice in a and d; the mass of the sample, 8;
is the mass of the standard sample, g;
w is the purity of the standard sample, % (m/m).
A7 Allowable difference
The difference between the results of two parallel determinations in this method should not exceed 1.0%. (A1)
Additional instructions:
HG2217-91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Wu Qi, Zhang Xuebing, Wang Yufan, Wang Shiyan, Wang Fengfengqin and Zheng Taiyong.2 Determination steps
Weigh 20g of the sample into a beaker and spread it into a smooth and uniform layer of equal thickness without using pressure. Place the metal block on the surface of the sample in the beaker. Store the beaker in an oven at 54±2℃ for 14 days. Take out the beaker, take out the round block, and cool it to room temperature in a desiccator without desiccant. Within 24 hours, test according to the methods specified in Articles 4.1, 4.3, and 4.5 of this standard. If the results meet the technical requirements of the standard, the thermal storage stability of the product is qualified. 5 Inspection rules
5.1 The wettable powder of thiophene should be inspected by the quality supervision and inspection department of the production unit. The production unit shall ensure that all wettable powders of thiophene leaving the factory meet the requirements of this standard. 5.2 The operating unit and the user unit have the right to inspect whether the wettable powder of thiophene received meets the requirements of this standard in accordance with the provisions of this standard.
5.3 The sampling method shall be carried out in accordance with GB1605. The sample should be divided into two bottles, one bottle is sent to the quality supervision and inspection department for inspection, and the other bottle is sealed. 5.4 In the test results, when there are indicators that do not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. In the re-test results, even if one indicator does not meet the requirements of this standard, the entire batch of Motujin wettable powder is an unqualified product. 5.5 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation between the two parties, or the statutory inspection agency can conduct arbitration analysis according to the inspection methods specified in this standard.
5.6 Under normal circumstances, the inspection cycle of type inspection items shall not exceed one quarter. 6 Marking, packaging, transportation and storage
6.1 Marking and packaging shall comply with the relevant provisions of GB3796. 6.2 During transportation and storage, it should be strictly prevented from moisture and sunlight, maintain good ventilation, and shall not be mixed with food, seeds, and feed. Avoid contact with the skin to prevent inhalation through the mouth and nose.
6.3 The warranty period of this product is two years. That is, under normal packaging and storage conditions, the content of quinolones should meet the technical requirements specified in this standard within two years from the date of leaving the factory.
A1 Method Summary
HG2217-91
Appendix A
Gas chromatography determination method for quinolones content
(Supplement)
The sample was dissolved in dimethylformamide, and simethoxazole was used as the internal standard. The quinolones were separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 60g simetholine dimethylformamide solution; Aminotriptyline standard sample: known content, >99% (m/m); simetholine: content ≥95% (m/m), no interferences after gas chromatography analysis; Gas chromatograph: with flame ionization detector; Chromatographic column: 2m long, 4mm inner diameter stainless steel column, filled with 5% XE-60/ChromosorbW/AW-DMCS (150~180um); Micro-injector: 10uL.
Chromatographic operating conditions
Temperature:
Column chamber 212℃;
Vaporization chamber 250℃;
Detector 250℃.
Gas flow rate:
Carrier gas (N)
20mL/min;
Hydrogen 30mL/min;
500mL/min.
Injection volume:
lμL.
Retention time:
Atrazine 7min;
Simethoine 11min.
The above chromatographic operating conditions are typical operating parameters. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect. A4 Preparation of standard solution and sample solution
HG221791
Figure A1 Gas chromatogram of Atrazine
1—Atrazine; 2—Simethoine
Weigh the standard and sample containing 0.08g of atrazine (accurate to 0.0001g) and place them in stoppered vials respectively. Use a pipette to transfer 2.0 mL of internal standard solution into each vial. Shake the vial thoroughly, let it stand, and take the supernatant for sampling. Centrifuge or filter if necessary. A5 Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the sirtuin standard solution until the relative deviation of the peak height ratio of sirtuin to sirtuin in two consecutive injections is less than 0.7%. Then inject in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
A6 Calculation
The mass percentage of squalane (ar) is calculated according to formula (A1): ism..w
In the formula, rs——the average value of the peak height ratio of squalane to squalane in the sample solution injected twice in b and c; rs——the average value of the peak height ratio of squalane to squalane in the standard solution injected twice in a and d; the mass of the sample, 8;
——the mass of the standard sample, g;
w——the purity of the standard sample, % (m/m).
A7 Allowable difference
The difference between the results of two parallel determinations in this method should not exceed 1.0%. (A1)
Additional instructions:
HG2217—91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Wu Qi, Zhang Xuebing, Wang Yufan, Wang Shiyan, Wang Fengfengqin and Zheng Taiyong.3 The warranty period of this product is two years. That is, under normal packaging and storage conditions, the content of quinolones should meet the technical requirements specified in this standard within two years from the date of leaving the factory.
A1 Method Summary
HG2217-91
Appendix A
Gas chromatography determination method for quinolones content
(Supplement)
The sample is dissolved in dimethylformamide, and simetropium is used as the internal standard. The quinolones are separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS chromatographic column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 60g simetholine dimethylformamide solution; Moxifen standard sample: known content, >99% (m/m); simetholine: content ≥95% (m/m), no interferences after gas chromatography analysis; Gas chromatograph: with flame ionization detector; Chromatographic column: 2m long, 4mm inner diameter stainless steel column, filled with 5% XE-60/ChromosorbW/AW-DMCS (150~180um); Micro-injector: 10uL.
Chromatographic operating conditions
Temperature:
Column chamber 212℃;
Vaporization chamber 250℃;
Detector 250℃.
Gas flow rate:
Carrier gas (N)
20mL/min;
Hydrogen 30mL/min;
500mL/min.
Injection volume:
lμL.
Retention time:
7min for atrazine;
11min for simethoprim.
The above chromatographic operating conditions are typical operating parameters. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect. A4 Preparation of standard solution and sample solution
HG221791
Figure A1 Gas chromatogram of atrazine
1—atrazine; 2—simethoprim
Weigh the standard and sample containing 0.08g atrazine (accurate to 0.0001g) and place them in stoppered vials respectively. Use a pipette to transfer 2.0 mL of internal standard solution into each vial. Shake the vial thoroughly, let it stand, and take the supernatant for sampling. Centrifuge or filter if necessary. A5 Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the sirtuin standard solution until the relative deviation of the peak height ratio of sirtuin to sirtuin in two consecutive injections is less than 0.7%. Then inject in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
A6 Calculation
The mass percentage of squalane (ar) is calculated according to formula (A1): ism..w
In the formula, rs——the average value of the peak height ratio of squalane to squalane in the sample solution injected twice in b and c; rs——the average value of the peak height ratio of squalane to squalane in the standard solution injected twice in a and d; the mass of the sample, 8;
——the mass of the standard sample, g;
w——the purity of the standard sample, % (m/m).
A7 Allowable difference
The difference between the results of two parallel determinations in this method should not exceed 1.0%. (A1)
Additional instructions:
HG2217—91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Wu Qi, Zhang Xuebing, Wang Yufan, Wang Shiyan, Wang Fengfengqin and Zheng Taiyong.3 The warranty period of this product is two years. That is, under normal packaging and storage conditions, the content of quinolones should meet the technical requirements specified in this standard within two years from the date of leaving the factory.
A1 Method Summary
HG2217-91
Appendix A
Gas chromatography determination method for quinolones content
(Supplement)
The sample is dissolved in dimethylformamide, and simetropium is used as the internal standard. The quinolones are separated and determined on a 5%XE-60/ChromosorbW/AW-DMCS chromatographic column.
Reagents and instruments
Dimethylformamide;
Internal standard solution: 60g simetholine dimethylformamide solution; Aminotriptyline standard sample: known content, >99% (m/m); simetholine: content ≥95% (m/m), no interferences after gas chromatography analysis; Gas chromatograph: with flame ionization detector; Chromatographic column: 2m long, 4mm inner diameter stainless steel column, filled with 5% XE-60/ChromosorbW/AW-DMCS (150~180um); Micro-injector: 10uL.
Chromatographic operating conditions
Temperature:
Column chamber 212℃;
Vaporization chamber 250℃;
Detector 250℃.
Gas flow rate:
Carrier gas (N)
20mL/min;
Hydrogen 30mL/min;
500mL/min.
Injection volume:
lμL.
Retention time:
Atrazine 7min;
Simethoine 11min.
The above chromatographic operating conditions are typical operating parameters. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect. A4 Preparation of standard solution and sample solution
HG221791
Figure A1 Gas chromatogram of Atrazine
1—Atrazine; 2—Simethoine
Weigh the standard and sample containing 0.08g of atrazine (accurate to 0.0001g) and place them in stoppered vials respectively. Use a pipette to transfer 2.0 mL of internal standard solution into each vial. Shake the vial thoroughly, let it stand, and take the supernatant for sampling. Centrifuge or filter if necessary. A5 Determination steps
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject the sirtuin standard solution until the relative deviation of the peak height ratio of sirtuin to sirtuin in two consecutive injections is less than 0.7%. Then inject in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
A6 Calculation
The mass percentage of squalane (ar) is calculated according to formula (A1): ism..w
In the formula, rs——the average value of the peak height ratio of squalane to squalane in the sample solution injected twice in b and c; rs——the average value of the peak height ratio of squalane to squalane in the standard solution injected twice in a and d; the mass of the sample, 8;
——the mass of the standard sample, g;
w——the purity of the standard sample, % (m/m).
A7 Allowable difference
The difference between the results of two parallel determinations in this method should not exceed 1.0%. (A1)
Additional instructions:
HG2217—91
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Wu Qi, Zhang Xuebing, Wang Yufan, Wang Shiyan, Wang Fengfengqin and Zheng Taiyong.
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