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WS/T 686-2020: (Detection methods and evaluation requirements of antiviral drugs in disinfectants and antibacterial agents)
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Basic data | Standard ID | WS/T 686-2020 (WS/T686-2020) | | Description (Translated English) | (Detection methods and evaluation requirements of antiviral drugs in disinfectants and antibacterial agents) | | Sector / Industry | Health Industry Standard (Recommended) | | Classification of Chinese Standard | C50 | | Word Count Estimation | 21,218 | | Date of Issue | 2020-07-20 | | Date of Implementation | 2021-02-01 | | Regulation (derived from) | State-health communication (2020) No. 14 | | Issuing agency(ies) | National Health Commission | WS/T 686-2020: (Detection methods and evaluation requirements of antiviral drugs in disinfectants and antibacterial agents)
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(Detection methods and evaluation requirements of antiviral drugs in disinfectants and antibacterial agents)
ICS 11.080
C 50
WS
People's Republic of China Health Industry Standard
Detection methods and evaluation requirements of antiviral drugs in disinfectants and antibacterial agents
Issued by the National Health Commission of the People's Republic of China
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
Drafting organizations of this standard. Beijing Municipal Center for Disease Control and Prevention, Chinese Academy of Metrology, Beijing Physical and Chemical Analysis and Testing Center, China
National Institute for Food and Drug Control, Jiangsu Provincial Center for Disease Control and Prevention, Chinese Center for Disease Control and Prevention, Shandong Provincial Center for Disease Control and Prevention.
The main drafters of this standard. Ding Xiaojing, Wang Ping, Yang Yi, Gao Yunhua, Zhao Xinlei, Gou Xinlei, Niu Xiameng, Li Li, Li Shuo, Li Jie,
Zhao Shan, Xu Yan, Li Fang, Zhang Liubo, Li Yan, Cui Shuyu, Su Guanmin.
Detection methods and evaluation requirements of antiviral drugs in disinfectants and antibacterial agents
1 Scope
This standard specifies the testing methods and evaluation requirements for antiviral drugs in disinfectants and antibacterial agents.
This standard applies to ganciclovir, acyclovir, penciclovir, ribavirin and other antiviral drugs in disinfectants and antibacterial agents
Measurement and evaluation.
2 Normative references
The following documents are indispensable for the application of this standard. For dated reference documents, only the dated version applies to this document.
For undated references, the latest version (including all amendments) applies to this document.
GB/T 6682 Analyze laboratory water specifications and test methods.
Pharmacopoeia of the People's Republic of China
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Antiviral drugs
Drugs used to prevent and treat viral infections.
4 Detection methods of ganciclovir, acyclovir and penciclovir
4.1 High performance liquid chromatography
4.1.1 Principle
The ganciclovir, acyclovir and penciclovir in the sample were ultrasonically extracted with a mixed solution of acetic acid and methanol, and the extract was centrifuged and filtered.
C18 column separation, UV detector or diode array detector detection, external standard method for quantification.
4.1.2 Reagents and materials
Unless otherwise specified, the reagents used in this method are all analytically pure, and the water is the first grade water specified in GB/T 6682.
4.1.2.1 Reagents
4.1.2.1.1 Methanol (CH3OH). chromatographically pure.
4.1.2.1.2 Glacial acetic acid (CH3COOH).
4.1.2.1.3 Ammonium acetate (CH3COONH4).
4.1.2.2 Reagent preparation
4.1.2.2.1 Sample extraction solution. Pipette 80 mL of methanol and 10 mL of glacial acetic acid respectively, place them in a reagent bottle, add 10 mL of water, and mix.
4.1.2.2.2 Ammonium acetate acetic acid buffer solution. Weigh 0.77 g of ammonium acetate, place it in a reagent bottle, add 400 mL of water to dissolve, and then add
2 mL of glacial acetic acid, add water to 500 mL, and mix well.
4.1.2.3 Standard product
The purity of ganciclovir, acyclovir and penciclovir are all greater than 97% or the standard substances certified and granted by the country. For other relevant information, see Appendix A.
4.1.2.4 Standard solution preparation
4.1.2.4.1 Standard stock solution. accurately weigh 25.0 mg each of ganciclovir, acyclovir and penciclovir, and place them in a 50 mL volume respectively
Add about 40 mL of sample extraction solution to the bottle, sonicate for 10 minutes, dissolve, dilute the volume with the sample extraction solution to the mark, and prepare the mass concentration
Both are 500 mg/L standard stock solutions. Keep refrigerated, the validity period is 3 months.
4.1.2.4.2 Mixed standard intermediate solution. Pipette the standard stock solutions of ganciclovir, acyclovir and penciclovir respectively, and extract the solution with the sample
Dilute into a mixed standard intermediate solution with a mass concentration of 50 mg/L. Keep refrigerated, valid for 1 month.
4.1.2.4.3 Mixed standard series solution. take different volumes of mixed standard intermediate solution and dilute with sample extraction solution to form mixed standard series
Solution, such as 0.5 mg/L, 2.5 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L. Now equipped for temporary use.
4.1.2.5 Materials
4.1.2.5.1 Organic filter membrane. the pore size is 0.45 m.
4.1.2.5.2 Glass beads. Φ< 5 mm.
4.1.3 Apparatus and equipment
4.1.3.1 High performance liquid chromatograph. with diode array detector or ultraviolet detector.
4.1.3.2 Analytical balance. the smallest division value is 0.1 mg.
4.1.3.3 Centrifuge. ≥3 000 r/min.
4.1.3.4 Vortex mixer.
4.1.3.5 Ultrasonic cleaner.
4.1.4 Analysis steps
4.1.4.1 Sample preparation
4.1.4.1.1 Liquid dosage form
Weigh 0.5 g (accurate to 1 mg) of the sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to 10 mL
Graduation, vortex and mix for 1 min, ultrasonic for 10 min, filter through a filter membrane, and set aside.
4.1.4.1.2 Other dosage forms
Weigh 0.5 g (accurate to 1 mg) sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to
10 mL scale, add 1 to 2 glass beads, vortex to mix until the solution is uniform, sonicate for 10 minutes, centrifuge for 5 minutes, and take the supernatant
Filter through a filter membrane and set aside.
4.1.4.2 HPLC reference conditions
The reference conditions of HPLC are as follows.
a) Chromatographic column. C18 column (column length 250 mm, inner diameter 4.6 mm, particle size 5 m), or equivalent;
b) Mobile phase. Phase A is methanol, phase B is ammonium acetate acetic acid buffer solution;
c) Flow rate. 1.0 mL/min;
d) Column temperature. 30℃;
e) Injection volume. 5 L;
f) Detection wavelength. 254 nm;
g) Gradient elution procedure. see Appendix B.1.
4.1.4.3 Preparation of standard curve
Inject the mixed standard series solutions into the high performance liquid chromatograph in order from low to high concentration, with the peak area of the chromatographic peak as the ordinate, and
The corresponding mass concentration is the abscissa, and the peak area-mass concentration (mg/L) standard curve is drawn. Ganciclovir, Acyclovir, and Penciclovir
Refer to Appendix C.1 for the high performance liquid chromatogram of Wei mixed standard solution.
4.1.4.4 Determination
The processed sample solution is injected into the high performance liquid chromatograph, and the mass concentration of the target compound in the sample solution is calculated according to the standard curve.
4.1.4.5 Calculation and expression of results
The content of the target compound in the sample is calculated according to formula (1).
4.1.4.6 Precision
The absolute difference between two independent determination results obtained under repeated conditions should not exceed 10% of the arithmetic mean. See Appendix D for the recovery rate and precision of this method.
4.1.4.7 Detection limit and quantification limit
When the sampling volume is 0.5 g and the constant volume is 10 mL, the detection limit and quantification limit of this method. ganciclovir, acyclovir and penciclovir
The detection limits are both 2.0 mg/kg; the quantification limits are both 7.0 mg/kg.
4.2 Micellar electrokinetic capillary chromatography
4.2.1 Principle
Extract ganciclovir, acyclovir and penciclovir in the sample with a sample extraction solution containing sodium lauryl sulfate, using micellar electrokinetic
Capillary chromatographic separation mode for separation, UV detector or diode array detector detection, external standard method for quantification.
4.2.2 Reagents and materials
Unless otherwise specified, the reagents used in this method are all analytically pure, and the water is the first-grade water specified in GB/T 6682.
4.2.2.1 Reagents
4.2.2.1.1 Sodium dodecyl sulfate (SDS, C12H25SO4Na).
4.2.2.1.2 Borax (Na2B4O7·10H2O).
4.2.2.1.3 Anhydrous sodium dihydrogen phosphate (NaH2PO4).
4.2.2.1.4 Sodium hydroxide (NaOH).
4.2.2.2 Reagent preparation
4.2.2.2.1 Separation buffer solution. weigh out 2.019 g of SDS, 0.191 g of borax and 0.150 g of anhydrous sodium dihydrogen phosphate and place them in the same container.
In a plastic centrifuge tube with a graduated stopper, add water to the 50 mL mark, dissolve and mix by ultrasonic, and prepare to contain 140 mmol/L SDS and 10 mmol/L
Separation buffer solution of borax and 25 mmol/L sodium dihydrogen phosphate.
4.2.2.2.2 Sample extraction solution. Dilute the separation buffer solution 10 times with water to prepare a sample extraction solution.
4.2.2.2.3 Sodium hydroxide solution. Weigh 2 g of sodium hydroxide, add it to a plastic centrifuge tube pre-filled with 40 mL of water, shake to dissolve,
Add water to the 50 mL mark, mix well, and prepare 1 mol/L sodium hydroxide solution.
4.2.2.3 Standard product
Same as 4.1.2.3.
4.2.2.4 Standard solution preparation
4.2.2.4.1 Standard stock solution. accurately weigh out 10.0 mg of ganciclovir, acyclovir and penciclovir, and place them in 10 mL volume respectively
Add about 5 mL of the sample extraction solution to the bottle, shake (or ultrasonic) to dissolve, dilute the volume with the sample extraction solution to the mark, and prepare a concentrated mass
The degree is 1000 mg/L standard stock solution. Now equipped for temporary use.
4.2.2.4.2 Mixed standard intermediate solution. Pipette the standard stock solutions of ganciclovir, acyclovir and penciclovir respectively, and extract the solution with the sample
Dilute into a mixed standard intermediate solution with a mass concentration of 100 mg/L. Now equipped for temporary use.
4.2.2.4.3 Mixed standard series solution. take different volumes of mixed standard intermediate solution and dilute with sample extraction solution to form mixed standard series
Solution, such as 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 40.0 mg/L. Now equipped for temporary use.
4.2.2.5 Materials
Same as 4.1.2.5.
4.2.3 Apparatus and equipment
4.2.3.1 Capillary electrophoresis instrument. with diode array detector or ultraviolet detector.
4.2.3.2 Uncoated fused silica capillary tube. inner diameter 50 m, outer diameter 375 m.
4.2.3.3 Same as 4.1.3.2.
4.2.3.4 Same as 4.1.3.4.
4.2.3.5 Same as 4.1.3.5.
4.2.4 Analysis steps
4.2.4.1 Sample pretreatment
4.2.4.1.1 Liquid dosage form
Weigh 0.5 g (accurate to 1 mg) of the sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to 10 mL
Mark, vortex and mix for 1 min, ultrasonic for 10 min, and set aside.
4.2.4.1.2 Other dosage forms
Weigh 0.5 g (accurate to 1 mg) of the sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to 10 mL
Graduation, add 1 to 2 glass beads, vortex and mix until the solution is uniform, sonicate for 10 min, and set aside.
4.2.4.2 Reference conditions for capillary electrophoresis
The reference conditions of capillary electrophoresis are as follows.
a) Separation column. uncoated fused silica capillary tube, 302 mm (effective length is.200 mm);
b) Voltage. 10 kV;
c) Injection pressure. 3.448 kPa;
d) Sampling time. 4 s (injection volume is about 7.9 nL);
e) Detection wavelength. 254 nm;
f) Cleaning procedure. before using the newly installed capillary, rinse with NaOH solution for 20 min and water for 5 min, and separate the buffer solution
Rinse for 5 minutes. Before each injection, rinse with NaOH solution for 1.5 min, water for 1.5 min, and separation buffer solution for 1.5 min.
4.2.4.3 Preparation of standard curve
Inject the mixed standard series solutions into the capillary electrophoresis apparatus in order of concentration from low to high, and divide the peak area by the chromatographic peak calibration peak area
Using migration time) as the ordinate, and its corresponding mass concentration as the abscissa, draw a calibration peak area-mass concentration (mg/L) standard curve.
Refer to Appendix E.1 for the capillary electrophoresis diagram of the mixed standard solution of ganciclovir, acyclovir and penciclovir.
4.2.4.4 Determination
The processed sample solution is injected into the capillary electrophoresis apparatus, and the mass concentration of the target compound in the sample solution is calculated according to the standard curve.
4.2.4.5 Calculation and expression of results
The content of the target compound in the sample is calculated according to formula (1).
The result retains three significant figures.
4.2.4.6 Precision
The absolute difference between two independent determination results obtained under repeated conditions should not exceed 10% of the arithmetic mean.
4.2.4.7 Detection limit and quantification limit
When the sampling volume is 0.5 g and the constant volume is 10 mL, the detection limit and quantification limit of this method. ganciclovir, acyclovir and penciclovir
The detection limit of Wei was 4.0 mg/kg; the limit of quantification was 14.0 mg/kg.
4.3 Confirmation method of ultra performance liquid chromatography-tandem mass spectrometry
4.3.1 Principle
Ultrasonic extraction of ganciclovir, acyclovir and penciclovir in the sample with a mixed solution of acetic acid and methanol, after centrifugation, filtration, and ultra-efficient
Liquid chromatography-tandem mass spectrometer for confirmation.
4.3.2 Reagents and materials
Unless otherwise specified, all reagents are analytically pure, and the water is first-grade water that meets the requirements of GB/T 6682.
4.3.2.1 Reagents
4.3.2.1.1 Methanol (CH3OH). chromatographically pure.
4.3.2.1.2 Formic acid (HCOOH). chromatographically pure.
4.3.2.1.3 Glacial acetic acid (CH3COOH).
4.3.2.2 Reagent preparation
4.3.2.2.1 Same as 4.1.2.2.1.
4.3.2.2.2 0.1% formic acid methanol solution. add 0.1 mL of formic acid to 100 mL of methanol and mix well.
4.3.2.2.3 0.1% formic acid aqueous solution. add 0.1 mL of formic acid to 100 mL of water and mix well.
4.3.2.3 Standard product
Same as 4.1.2.3.
4.3.2.4 Standard solution preparation
4.3.2.4.1 Same as 4.1.2.4.1.
4.3.2.4.2 Mixed standard intermediate solution. Pipette the standard stock solutions of ganciclovir, acyclovir and penciclovir respectively, and dissolve them with water to form a concentrated mass
The concentration is 5 mg/L mixed standard intermediate solution. Keep refrigerated, valid for 1 month.
4.3.2.4.3 Mixed standard application solution. Dilute the mixed standard intermediate solution 100 times with water to prepare a mixture with a mass concentration of 50 g/L
Standard application fluid. Now equipped for temporary use.
4.3.2.5 Materials
4.3.2.5.1 Organic filter membrane. the pore size is 0.22 m.
4.3.2.5.2 Same as 4.1.2.5.2.
4.3.3 Apparatus and equipment
4.3.3.1 Ultra performance liquid chromatography-tandem mass spectrometer. charged ion source.
4.3.3.2 Same as 4.1.3.2.
4.3.3.3 Same as 4.1.3.3.
4.3.3.4 Same as 4.1.3.4.
4.3.3.5 Same as 4.1.3.5.
4.3.4 Analysis steps
4.3.4.1 Sample preparation
4.3.4.1.1 Liquid dosage form
Weigh 0.5 g (accurate to 1 mg) sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to
10 mL mark, vortex and mix for 1 min, ultrasonic for 10 min, filter through a filter membrane, dilute the filtrate at least 10 times with water, mix well, and set aside.
4.3.4.1.2 Other dosage forms
Weigh 0.5 g (accurate to 1 mg) sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to
Add 1 to 2 glass beads to a 10 mL scale, vortex to mix until the solution is uniform, sonicate for 10 minutes, centrifuge for 5 minutes, and supernatant
Filter through a membrane, dilute the filtrate at least 10 times with water, mix well, and set aside.
4.3.4.2 UHPLC reference conditions
The reference conditions of ultra performance liquid chromatography are as follows.
a) Chromatographic column. C18 (column length 50 mm, inner diameter 2.1 mm, particle size 1.7 m), or equivalent;
b) Mobile phase. Phase A is 0.1% formic acid methanol solution; Phase B is 0.1% formic acid aqueous solution;
c) Flow rate. 0.3 mL/min;
d) Column temperature. 40℃;
e) Injection volume. 5 L;
f) Gradient elution procedure. see Appendix B.2.
4.3.4.3 Reference conditions for mass spectrometry
The mass spectrometry reference conditions are as follows.
a) Ionization method. ESI;
b) Desolventizing gas temperature. 350℃;
c) Dry air flow rate. 550 L/h;
d) Collision gas flow rate. 0.15 mL/min;
e) Capillary voltage. 3.5 kV;
f) Monitoring mode. multiple reaction monitoring (MRM) mode;
g) Other mass spectrometry parameters. see Appendix F.1.
4.3.4.4 Determination of mixed standard application solution
Inject the mixed standard application solutions of 50 g/L into the ultra performance liquid chromatography-tandem mass spectrometer. For the mass spectrogram chromatogram, see Appendix C.2.
4.3.4.5 Confirmation
The processed sample solution is injected into the ultra-high performance liquid chromatography-tandem mass spectrometer. Under the same test conditions, the color of the target compound in the sample
The retention time of the peak is compared with the retention time of the corresponding standard chromatographic peak, the variation range should be within ±2.5%, and the detected ion is relatively
The abundance should be consistent with the relative ion abundance in the standard solution of equivalent concentration. The relative abundance ratio deviation should meet the requirements of Table 1.
Table 1 Maximum allowable deviation of relative ion abundance
Relative ion abundance (A, %) ＞50 20A≤50 10A≤20 ≤10
Maximum allowable deviation (%) ±20 ±25 ±30 ±50
4.3.4.6 Detection limit
When the sampling volume is 0.5 g and the constant volume is 10 mL, the detection limit of this method. ganciclovir, acyclovir and penciclovir are all 20.0 g/kg.
5 Detection method of ribavirin
5.1 Capillary electrophoresis with electroosmotic flow reversal
5.1.1 Principle
The ribavirin in the sample was extracted with a sample extraction solution containing boric acid and borax, and the electroosmotic flow reversed zone electrophoresis separation mode was used for separation
Separation, UV detector or diode array detector detection, external standard method quantification.
5.1.2 Reagents and materials
Unless otherwise specified, all reagents are analytically pure, and the water is first-grade water that meets the requirements of GB/T 6682.
5.1.2.1 Reagents
5.1.2.1.1 Boric acid (H3BO3).
5.1.2.1.2 Borax (Na2B4O7·10H2O).
5.1.2.1.3 Cetyltrimethylammonium bromide (CTAB, C19H42BrN).
5.1.2.1.4 Sodium hydroxide (NaOH).
5.1.2.2 Reagent preparation
5.1.2.2.1 Separation buffer solution. weigh 0.309 g of boric acid, 1.144 g of borax and 0.009 g of CTAB, and place them on the same scale with a stopper.
In a plastic centrifuge tube, add about 40 mL of water and shake to dissolve, then add water to the 50 mL mark, mix well, and prepare to contain 100 mmol/L boric acid,
A separation buffer solution of 60 mmol/L borax and 0.5 mmol/L CTAB.
5.1.2.2.2 Sample extraction solution. Dilute the separation buffer solution 10 times with water to prepare a sample extraction solution.
5.1.2.2.3 Same as 4.2.2.2.3.
5.1.2.3 Standard product
Ribavirin is a standard substance whose purity is greater than 97% or has been certified and granted a certificate by the country. For other relevant information, see Appendix A.
5.1.2.4 Standard solution preparation
5.1.2.4.1 Standard stock solution. accurately weigh 10.0 mg of ribavirin, place it in a 10 mL volumetric flask, add about 5 mL of water and shake to dissolve it.
Then dilute the volume to the mark with water and prepare a standard stock solution with a mass concentration of 1000 mg/L. Keep refrigerated, the validity period is 3 months.
5.1.2.4.2 Standard intermediate solution. Dilute the ribavirin standard stock solution with the sample extraction solution 10 times to prepare a mass concentration of 100
Standard intermediate solution of mg/L. Now equipped for temporary use.
5.1.2.4.3 Standard series solution. take different volumes of ribavirin standard intermediate solution and dilute with sample extraction solution to form a mixed standard series
Solution, such as 1.5 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 50.0 mg/L. Now equipped for temporary use.
5.1.2.5 Materials
Same as 4.1.2.5.2.
5.1.3 Apparatus and equipment
5.1.3.1 Capillary electrophoresis instrument. with diode array detector or ultraviolet detector.
5.1.3.2 Uncoated fused silica capillary tube. inner diameter 50 m, outer diameter 375 m.
5.1.3.3 Same as 4.1.3.2.
5.1.3.4 Same as 4.1.3.4.
5.1.3.5 Same as 4.1.3.5.
5.1.4 Analysis steps
5.1.4.1 Sample preparation
5.1.4.1.1 Liquid dosage form
Weigh 0.5 g (accurate to 1 mg) of the sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to 10 mL
Mark, vortex and mix for 1 min, ultrasonic for 10 min, and set aside.
5.1.4.1.2 Paste dosage form
Weigh 0.2 g (accurate to 1 mg) of the sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to 10 mL
Graduation, add 1 to 2 glass beads, vortex and mix until the solution is uniform, sonicate for 10 min, and set aside.
5.1.4.1.3 Other dosage forms
Weigh 0.5 g (accurate to 1 mg) of the sample into a 10 mL centrifuge tube (colorimetric tube) with a stopper and add the sample extraction solution to 10 mL
Graduation, add 1 to 2 glass beads, vortex and mix until the solution is uniform, sonicate for 10 min, and set aside.
5.1.4.2 Reference conditions for capillary electrophoresis.
a) Uncoated fused silica capillary tube, 700 mm (effective length is 600 mm);
b) Voltage. 29 kV;
c) Injection pressure. 3.448 kPa;
d) Sampling time. 20 s (injection volume is about 17 nL);
e) Detection wavelength. 214 nm;
f) Cleaning procedure. before using the newly installed capillary, rinse with NaOH solution for 20 min and water for 5 min, and separate the buffer solution
Rinse for 5 minutes. Before each injection, rinse with NaOH for 1.5 min, water for 1.5 min, and separation buffer solution for 1.5 min.
5.1.4.3 Preparation of standard curve
Inject the standard series solutions into the capillary electrophoresis apparatus in order of concentration from low to high, and use the corrected peak area of the chromatographic peak (the peak area divided by the shift
Shift time) is the ordinate, and the corresponding mass concentration is the abscissa, draw a calibration peak area-mass concentration (mg/L) standard curve. Profit
The capillary electrophoresis diagram of bavirin standard solution is shown in Appendix E.2.
5.1.4.4 Determination
The processed sample solution is injected into the capillary electrophoresis apparatus, and the mass concentration of ribavirin in the sample solution is calculated according to the standard curve.
5.1.4.5 Calculation and expression of results
The content of ribavirin in the sample is calculated according to formula (1).
The result retains three significant figures.
5.1.4.6 Precision
The absolute difference between two independent determination results obtained under repeated conditions should not exceed 10% of the arithmetic mean.
5.1.4.7 Detection limit and quantification limit
Paste sample. when the sampling volume is 0.20 g, the constant volume is 10 mL, the detection limit of this method is 20 mg/kg, and the quantification limit is 70 mg/kg;
Other samples. When the sampling volume is 0.50 g and the constant volume is 10 mL, the detection limit of this method is 8 mg/kg, and the quantification limit is 30 mg/kg.
5.2 Confirmation method of ultra performance liquid chromatography-tandem mass spectrometry
5.2.1 Principle
The ribavirin in the sample was ultrasonically extracted with a methanol-water mixed solution, purified by a C18-solid phase extraction column, and confirmed by ultra-high performance liquid chromatography-tandem mass spectrometer.
5.2.2 Reagents and materials
Unless otherwise specified, all reagents are analytically pure, and the water is first-grade water that meets the requirements of GB/T 6682.
5.2.2.1 Reagents
5.2.2.1.1 Methanol (CH3OH). chromatographically pure.
5.2.2.1.2 Formic acid (HCOOH). chromatographically pure.
5.2.2.1.3 Acetonitrile (CH3CN). chromatographically pure.
5.2.2.2 Reagent preparation
5.2.2.2.1 Sample extraction solution. m...
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