Chinese Journal of Chromatography ›› 2025, Vol. 43 ›› Issue (2): 197-203.DOI: 10.3724/SP.J.1123.2024.03012
• Teaching Research • Previous Articles
ZHAO Ran, ZHANG Ling, ZHANG Kun, LI Youxin*(
)
Received:2024-03-14
Online:2025-02-08
Published:2025-01-23
Supported by:CLC Number:
ZHAO Ran, ZHANG Ling, ZHANG Kun, LI Youxin. Reform and exploration of the experimental teaching mode of teaching assistant and group rotation system: taking pharmaceutical analysis experiment course as an example[J]. Chinese Journal of Chromatography, 2025, 43(2): 197-203.
| Exp. No. | Peking University[ | Jiangsu Normal University[ | Nanjing Agricultural University[ |
|---|---|---|---|
| 1 | introduction to experiments in drug analysis | use and maintenance of pH meter (optional) | basic knowledge for drug analysis experiments |
| 2 | glucose impurity check | determination of the absorption coefficients of drugs | preparation and calibration of perchloric acid standard solutions |
| 3 | drug impurity evaluation | effect of GC carrier gas flow rate and column temperature on separation (optional) | general impurity check for glucose |
| 4 | determination of amiodarone content | selection of HPLC conditions (optional) | calibration of iodine standard solutions and determination of vitamin content |
| 5 | extraction and titration of procaine hydrochloride injection | inspection of drug impurities | determination of fluorenone-related substances at high and low concentrations using thin layer chromatography |
| 6 | determination of atropine sulfate injection | determination of lidocaine hydrochloride content | inspection of drug impurities |
| 7 | determination of ethamsylate injection | identification of ibuprofen using ultraviolet spectrophotometry and infrared spectroscopy (optional) | determination of vitamin A content in vitamin AD capsules using three-point correction |
| 8 | determination of methyl isoxazole and trimethoprim in compound sulfamethoxazole tablets using dual-wavelength spectrophotometry | analysis of procaine hydrochloride injection | determination of florfenicol content using HPLC |
| 9 | determination of the content of compound acetylsalicylic acid tablets | determination of vitamin E capsules using GC | determination of ethanol content in tinctures |
| 10 | determination of salicylic acid content in aspirin capsules | ||
| 11 | determination of penicillin sodium content for drug injection | ||
| 12 | determination of vitamin B1 content in tablets using differential spectrophotometry | ||
| Total time | 48 h | 48 h | 27 h |
Table 1 Experimental contents of pharmaceutical analysis experiment courses in some domestic colleges and universities
| Exp. No. | Peking University[ | Jiangsu Normal University[ | Nanjing Agricultural University[ |
|---|---|---|---|
| 1 | introduction to experiments in drug analysis | use and maintenance of pH meter (optional) | basic knowledge for drug analysis experiments |
| 2 | glucose impurity check | determination of the absorption coefficients of drugs | preparation and calibration of perchloric acid standard solutions |
| 3 | drug impurity evaluation | effect of GC carrier gas flow rate and column temperature on separation (optional) | general impurity check for glucose |
| 4 | determination of amiodarone content | selection of HPLC conditions (optional) | calibration of iodine standard solutions and determination of vitamin content |
| 5 | extraction and titration of procaine hydrochloride injection | inspection of drug impurities | determination of fluorenone-related substances at high and low concentrations using thin layer chromatography |
| 6 | determination of atropine sulfate injection | determination of lidocaine hydrochloride content | inspection of drug impurities |
| 7 | determination of ethamsylate injection | identification of ibuprofen using ultraviolet spectrophotometry and infrared spectroscopy (optional) | determination of vitamin A content in vitamin AD capsules using three-point correction |
| 8 | determination of methyl isoxazole and trimethoprim in compound sulfamethoxazole tablets using dual-wavelength spectrophotometry | analysis of procaine hydrochloride injection | determination of florfenicol content using HPLC |
| 9 | determination of the content of compound acetylsalicylic acid tablets | determination of vitamin E capsules using GC | determination of ethanol content in tinctures |
| 10 | determination of salicylic acid content in aspirin capsules | ||
| 11 | determination of penicillin sodium content for drug injection | ||
| 12 | determination of vitamin B1 content in tablets using differential spectrophotometry | ||
| Total time | 48 h | 48 h | 27 h |
| Exp. No. | Title | Purposes | Assay method |
|---|---|---|---|
| 1 | determination of the melting points of aspirin, artemether, and their derivatives | understand the definition of melting point; master the melting point determination method and its application in the field of drug research | melting point method |
| 2 | spectrophotometric determination of aspirin, artemether, and their derivatives | master the principle of polarimetric analysis for drug determination | polarimetry |
| 3 | identification of aspirin, artemether, and their derivatives using colorimetry | master the method of drug identification using colorimetry | colorimetry |
| 4 | identification of aspirin, artemether, and their derivatives using thin layer chromatography | master the method of drug identification using thin layer chromatography | thin layer chromatography |
| 5 | identification of aspirin, artemisinin, and their derivatives using infrared spectroscopy | master the principle and method of drug identification using infrared spectroscopy | infrared spectroscopy |
| 6 | identification of aspirin, artemisinin, and their derivatives using ultraviolet spectrophotometry | master the principle and method of drug identification using ultraviolet spectrophotometry | ultraviolet spectrophotometry |
Table 2 Identification tests of drugs
| Exp. No. | Title | Purposes | Assay method |
|---|---|---|---|
| 1 | determination of the melting points of aspirin, artemether, and their derivatives | understand the definition of melting point; master the melting point determination method and its application in the field of drug research | melting point method |
| 2 | spectrophotometric determination of aspirin, artemether, and their derivatives | master the principle of polarimetric analysis for drug determination | polarimetry |
| 3 | identification of aspirin, artemether, and their derivatives using colorimetry | master the method of drug identification using colorimetry | colorimetry |
| 4 | identification of aspirin, artemether, and their derivatives using thin layer chromatography | master the method of drug identification using thin layer chromatography | thin layer chromatography |
| 5 | identification of aspirin, artemisinin, and their derivatives using infrared spectroscopy | master the principle and method of drug identification using infrared spectroscopy | infrared spectroscopy |
| 6 | identification of aspirin, artemisinin, and their derivatives using ultraviolet spectrophotometry | master the principle and method of drug identification using ultraviolet spectrophotometry | ultraviolet spectrophotometry |
| Exp. No. | Title | Purposes | Assay methods |
|---|---|---|---|
| 7 | determination of impurities in aspirin and artemether | learn methods for impurity determination in drugs | colorimetry, precipitation method, loss-on-drying method |
| 8 | determination of aspirin, artemether, and related substances using HPLC | master the principle and method of drug impurity detection using HPLC; become familiar with the working principle and operation of HPLC; understand routine HPLC maintenance | aspirin: HPLC and one-point external standard method; artemether: HPLC and self-comparison method |
Table 3 Impurity inspection tests
| Exp. No. | Title | Purposes | Assay methods |
|---|---|---|---|
| 7 | determination of impurities in aspirin and artemether | learn methods for impurity determination in drugs | colorimetry, precipitation method, loss-on-drying method |
| 8 | determination of aspirin, artemether, and related substances using HPLC | master the principle and method of drug impurity detection using HPLC; become familiar with the working principle and operation of HPLC; understand routine HPLC maintenance | aspirin: HPLC and one-point external standard method; artemether: HPLC and self-comparison method |
| Exp. No. | Title | Purpose | Quantitative methods |
|---|---|---|---|
| 9 | determination of aspirin using HPLC | learn the principle of HPLC for drug analysis applications; learn the method of aspirin content determination using HPLC | HPLC and standard curve method |
| 10 | determination of aspirin using titration and ultraviolet spectrophotometry | master the titration method for determining aspirin content; master the ultraviolet spectrophotometry method for determining aspirin content; in combination with experiment No. 9, compare the differences, advantages and disadvantages, and limitations of the three methods for determining aspirin content | titration method (from Chinese Pharmacopoeia), ultraviolet spectrophotometry method (self-developed) |
| 11 | determination of artemether using HPLC | master the HPLC method for artemether determination; learn about the relationship between detection wavelength and the structure of artemether | HPLC and standard curve method |
Table 4 Determination tests of drug content
| Exp. No. | Title | Purpose | Quantitative methods |
|---|---|---|---|
| 9 | determination of aspirin using HPLC | learn the principle of HPLC for drug analysis applications; learn the method of aspirin content determination using HPLC | HPLC and standard curve method |
| 10 | determination of aspirin using titration and ultraviolet spectrophotometry | master the titration method for determining aspirin content; master the ultraviolet spectrophotometry method for determining aspirin content; in combination with experiment No. 9, compare the differences, advantages and disadvantages, and limitations of the three methods for determining aspirin content | titration method (from Chinese Pharmacopoeia), ultraviolet spectrophotometry method (self-developed) |
| 11 | determination of artemether using HPLC | master the HPLC method for artemether determination; learn about the relationship between detection wavelength and the structure of artemether | HPLC and standard curve method |
 |
Table 5 Schematic of the rotation mechanism
| |
| Instrument | Model | Number | Number of experiments involved | Average time per student/h |
|---|---|---|---|---|
| Polarimeter | Anton Paar, MCP 200 | 1 | 1 | 1 |
| Ultraviolet spectrophotometer | Agilent, Cary 60 | 9 | 3 | 4 |
| Fourier transform infrared spectrometer | Bruker, TENSOR 27 | 1 | 1 | 1 |
| HPLC | Agilent, 1220/1260 | 2 | 2 | 4 |
| Liquid chromatograph-mass spectrometer | Waters, Acquity RDa | 1 | 1 | 1 |
| UPLC | Bruker, micrOTOF-Q II | 1 | 1 | 1 |
| NMR spectrometer | Bruker, AVANCE III, 600 MHz | 1 | extension | 0.2 |
Table 6 List of large instruments
| Instrument | Model | Number | Number of experiments involved | Average time per student/h |
|---|---|---|---|---|
| Polarimeter | Anton Paar, MCP 200 | 1 | 1 | 1 |
| Ultraviolet spectrophotometer | Agilent, Cary 60 | 9 | 3 | 4 |
| Fourier transform infrared spectrometer | Bruker, TENSOR 27 | 1 | 1 | 1 |
| HPLC | Agilent, 1220/1260 | 2 | 2 | 4 |
| Liquid chromatograph-mass spectrometer | Waters, Acquity RDa | 1 | 1 | 1 |
| UPLC | Bruker, micrOTOF-Q II | 1 | 1 | 1 |
| NMR spectrometer | Bruker, AVANCE III, 600 MHz | 1 | extension | 0.2 |
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