31 August 2025, Volume 45 Issue 8
    

  • Select all
    |
    Review & Monography
  • Research progress on chiral stationary phase for chiral resolution of flavonoid compounds*
    ZHANG Guo-qiong, ZHONG Yue-tong, LI Lin-zhe, YANG Ze-rong, ZHANG Mei
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1287-1298. https://doi.org/10.16155/j.0254-1793.2024-1248
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Pharmacological studies have demonstrated the important role of flavonoids in promoting human health. The determination of pharmacological activity requires using of monomeric compounds. However, the advancement of precision medicine has imposed more stringent requirements on compounds, especially compounds intended for therapeutic use. In chiral drug research, the impact of optical isomers on drug efficacy should not be overlooked. While most drugs are used in clinical practice as racemates, certain isomers may not only reduce therapeutic efficacy, but increase metabolic load or even cause toxicity. Chiral stationary phases (CSP) are important materials for obtaining optically pure flavonoid compounds and represent a core aspect of chiral research. This review summarizes the recent developments in chiral stationary phases for the enantioseparation of flavonoids, in order to provide a reference for the chiral separation of flavonoids and offer new perspectives for further exploration and utilization of flavonoid compounds.
    • Ingredient Analysis
  • Determination of 16 saponins in compound Sanqi capsules by UPLC-MS/MS*
    HONG Fang, LIN Chen, ZHUANG Shan-shan, LIN Long, ZHOU Lin, LIN Si-rong, HUANG Ming-qing
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1299-1310. https://doi.org/10.16155/j.0254-1793.2025-0030
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To develop an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of 16 saponins (notoginsenoside R1, notoginsenoside Fa, notoginsenoside Fe, ginsenoside Re, ginsenoside Rg1, ginsenoside Rf, ginsenoside F3, ginsenoside Rg2, ginsenoside Rb1, ginsenoside F1, ginsenoside Rb2, ginsenoside Rb3, ginsenoside Rd, ginsenoside F2, ginsenoside Rg5, and 20(S)-ginsenoside Rg3) in compound Sanqi capsules, and to evaluate the quality of these compound Sanqi capsules. Methods: The samples were extracted with methanol using ultrasonic extraction, and separation was performed on a Thermo Fisher Scientific Accucore Phenyl Hexyl column (2.1 mm×100 mm, 2.6 µm) using gradient elution, with 0.1% formic acid aqueous solution (A) and acetonitrile (B) as mobile phase. The flow rate was 0.4 mL · min-1, the column temperature was 35 ℃, and the injection volume was 2 μL. Mass spectrometry was performed by using a heated electrospray ion source (HESI), and parallel reaction monitoring (PRM) in negative ion mode was employed for data acquisition and determination. The spray voltage was 2.8 kV(-). Results: The established method showed a good linear relationship within a certain concentration range (r≥0.997 0). The precision, repeatability and stability of the tested samples were good with recoveries ranging from 96.6% to 102.3%, and the RSDs between 1.1% and 5.1%. The results indicated that the contents of the 16 saponins were different among samples from different manufacturers and different batches of samples from the same manufacturer. The average total saponin contents of the samples from the three manufacturers were 33 019.650 8, 32 801.840 8, and 27 108.822 0 μg · g-1 respectively. Among the 10 batches of samples, the one with the lowest content was ginsenoside Rf and the top five saponin components in terms of content were ginsenoside Rg1, ginsenoside Rb1, notoginsenoside R1, ginsenoside Rd, and ginsenoside Re in sequence. Moreover, the average total contents of these five saponins all accounted for more than 95% of the total saponins, and could be used as markers that contribute significantly to quality differences. Additionally, cluster analysis could be divided into 3 categories according to manufacturers. Statistics showed that in the samples classified by cluster analysis as class Ⅰ, the dispersion degrees of the other saponins in the box diagram were greater than thoes in class Ⅱ and class Ⅲ. except ginsenoside Rb2 and contents of ginsenoside Rg5 were significantly higher than those in class Ⅱ and class Ⅲ, with a significant difference (P<0.001). The qualities of 3 batches of samples in class Ⅱ were stable, and contents of ginsenoside Rb2 were significantly different from those in class Ⅰ and class Ⅲ (P<0.001). The components of saponins in class Ⅲ samples were lower than those in class Ⅰ and class Ⅱ samples. Conclusion: The method can quickly, efficiently and accurately determine the contents of 16 saponins in compound Sanqi capsules, and provides a reference for the quality control of compound Sanqi capsules.
  • Comparison of the chemical components in different botanical parts of Artemisia stolonifera by GC-Q TOF MS/MS*
    CAO Ye, REN Yan, XU Yang, ZHENG Ling-ling, CHANG Na-na, WANG Ye, LI Hui
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1311-1319. https://doi.org/10.16155/j.0254-1793.2025-0085
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To compare the moxa yield and chemical components in different botanical parts of Artemisia stolonifera. Methods: The moxa yield of leaves on the middle stem (L), young leaves on the lateral branch (SL), inflorescences (F), non-lignified stems (S) and lignified stems (OS) of A. stolonifera were determined,and the chemical components were identified and analyzed by gas chromatography-quadrupole-time-of-flight tandem mass spectrometry (GC-Q TOF MS/MS). Principal component analysis (PCA), partial least squares-discriminant analysis (PLS-DA) and variable importance in projection (VIP) were used to find the characteristic components of A. stolonifera. Results: The highest moxa yield was obtained from the young leaves on lateral branches of A. stolonifera. A total of 19 compounds were detected, with terpenoids being the predominant class. Among the five botanical parts, six common volatile components were identified, which were β-caryophyllene, humulene, germacrene D, bicyclogermacrene, spathulenol, and caryophyllene oxide. Cluster heatmap revealed that L and S groups clustered together, whereas the F, SL, and OS formed another cluster. PLS-DA analysis pinpointed 6 components that significantly contributed to the differentiation among various botanical parts of A. stolonifera. Conclusion: Variations in the moxa yield, chemical constituents, and the contents of volatile components are observed among different botanical parts, which provides theoretical and data references for the further development and application of A. stolonifera.
  • Simultaneous determination of 9 components in Yiqing tablets by QAMS
    LI Xue-jiao, ZHANG Jia-yi, ZHANG Yu-meng, LIU Guo-hua, ZHAO Chun-jie, ZHAO Min
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1320-1330. https://doi.org/10.16155/j.0254-1793.2024-1242
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To simultaneously determine the contents of baicalin, berberine hydrochloride, baicalein, wogonin, aloe-emodin, emodin, rhein, chrysophanol and physcion in Yiqing tablets using the quantitative analysis of multi-components by single-marker (QAMS) method. Methods: The HPLC method was employed using an Ultimate® AQ-C18 column (4.6 mm×250 mm, 5 μm) with a mobile phase of 0.1% phosphoric acid aqueous solution (A)-acetonitrile (B) in gradient elution mode. The analysis was performed at a flow rate of 0.8 mL · min-1, detection wavelength of 265 nm, column temperature of 30 ℃, and injection volume of 10 μL. Baicalin served as the reference substance for calculating the relative correction factors (RCFs) and determining the contents of the other eight components. Results: Baicalin, berberine hydrochloride, baicalein, wogonin, aloe emodin, emodin, rhein, emodin and emodin methyl ether showed good linear relationships within their respective ranges (r≥0.999 0), with average recovery rates of 95%-110% and RSD<5%. The relative correction factors for berberine hydrochloride, baicalein, baicalein, aloe emodin, emodin, rhein, chrysophanol and emodin methyl ether were 1.71, 1.88, 0.63, 0.78, 0.74, 1.15, 0.80, and 3.65, respectively. The results obtained by QAMS method and external standard method were close to each other. The contents determined by the one QAMS method were 11.93, 6.760, 1.049, 0.135 1, 0.131 6, 0.606 0, 0.153 3 and 0.580 0 mg · g-1, respectively. Conclusion: This method has good specificity, high accuracy, stability and reliability, and can be used for quality control of Yiqing tablets.
  • Establishment of national standards for valproic acid, phenytoin and phenobarbital in frozen human serum*
    YU Ting, SHEN Min, ZHANG Juan-li, SUN Nan
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1331-1337. https://doi.org/10.16155/j.0254-1793.2025-0021
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To establish national standards for valproic acid, phenytoin and phenobarbital in frozen human serum. Methods: Anticoagulated human serum with a clear appearance, free from visible jaundice, lipemia and hemolysis, and testing negative for four infectious diseases was collected. After three-stage filtration, pure valproic acid, phenytoin, and phenobarbital were added to prepare two target concentrations. The mixtures were thoroughly homogenized and aliquoted to produce two levels of reference standards. The reference method (isotope-dilution liquid chromatography-tandem mass spectrometry) was used to determine the values of the reference standards. Homogeneity, stability, and uncertainty were evaluated in accordance with the national metrological technical specification JJF 1343-2022 Characterization, Homogeneity, and Stability Assessment of Reference Materials. Commutability was evaluated according to the WS/T 356-2024 Guideline for evaluation of commutability of reference materials. Results: The F values from the homogeneity tests for standard level 1 of valproic acid, phenytoin, and phenobarbital were 1.466 5, 1.475 9, and 1.439 4, respectively. The F values for standard level 2 were 1.334 8, 1.282 6, and 1.455 3, respectively. All values were less than F0.05 (1.511 7), indicating no significant differences. Standard levels 1 and 2 were stable for at least 30 d under storage conditions of (20-25) ℃, (2-8) ℃, and -20 ℃. The assigned values (k=2) for standard level 1 were: valproic acid (24.7±2.3) μg · mL-1, phenytoin (4.9±0.4) μg · mL-1, phenobarbital (5.0±0.4) μg · mL-1. For standard level 2: valproic acid (77.8±3.2) μg · mL-1, phenytoin (17.5±0.7) μg · mL-1, phenobarbital (34.6±1.6) μg · mL-1. The commutability results of the standards in two conventional testing systems met the requirements. Conclusion: This batch of frozen human serum national reference standards for valproic acid, phenytoin, and phenobarbital demonstrates accurate assigned values, good homogeneity and stability, and satisfactory commutability. After being made publicly available, it can be used for calibration and accuracy verification of detection reagents for valproic acid, phenytoin, and phenobarbital in serum. It is expected to play an important role in promoting the standardization and harmonization of test results.
  • Establishment of the first batch of national reference standard for sertraline hydrochloride impurity Ⅱ*
    ZHAO Wen, NI Xue, LI Li, LI Li, ZHOU Xiao-li, YIN Li-hui
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1338-1346. https://doi.org/10.16155/j.0254-1793.2025-0014
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To develop the first batch of national reference standard for sertraline hydrochloride impurity Ⅱ, which will be used for quality control of sertraline hydrochloride tablets, capsules and related products, in order to ensure the medication safety for patients. Methods: The structure of sertraline hydrochloride impurity Ⅱ was confirmed by LC-MS and nuclear magnetic resonance (NMR). Its absolute configuration was determined using ECD. HPLC was employed for purity analysis. The content of sertraline hydrochloride impurity Ⅱ was calculated using the mass balance method, with qNMR used for supplementary quantification. Results: The structure of the first batch of national reference standard for sertraline hydrochloride impurity Ⅱ was characterized, and its content was determined to be 99.7%. Conclusion: The first batch of national reference standard for sertraline hydrochloride impurity Ⅱ was established to meet the requirements for impurity identification in system suitability tests, as specified in the national standards for related drug products.
    • Metabolism Analysis·Bioassay
  • Exploring the effect of alisol G on lipid metabolism during differentiation of 3T3-L1 preadipocytes based on UPLC-Q TOF-MS/MS*
    SU Dai-feng, ZHANG Hong-yan, ZHOU Jie, LIN Ya-juan, GUO Lin-juan, ZENG Xue-jin, CHEN Quan-cheng, ZHANG Wei-yun
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1347-1359. https://doi.org/10.16155/j.0254-1793.2024-1140
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To investigate the effect of alisol G (AG) on lipid metabolism during 3T3-L1 preadipocyte differentiation. Methods: The differentiation of 3T3-L1 preadipocytes was induced by a combination of insulin, 3-isobutyl-1-methylxanthine, and dexamethasone. AG was added to mediate the process. Oil red O staining method was performed after intervention with AG. The contents of the relative lipid, triglyceride (TG) and total cholesterol (TC) within the cells were determined. Ultra performance liquid chromatography-quadrupole-time of flight-tandem mass spectrometry (UPLC-Q TOF-MS/MS) techniques were adopted to analyze changes in the lipid profile and the impact of lipid metabolism pathways. Results: The contents of lipid, TG, and TC during the differentiation process of 3T3-L1 preadipocytes were significantly reduced by 5 mol · L-1 and 10 mol · L-1 AG (P<0.01). After cellular lipidomics analysis, potential differential lipid metabolites were mainly fatty acid (FA) and glycerophosphatide (GP). KEGG enrichment analysis showed that AG affected the differentiation of 3T3-L1 preadipocytes mainly through Biosynthesis of unsaturated fatty acids, glycosylphosphatidylinositol (GPI)-anchor biosynthesis, glycerophospholipid metabolism and other metabolic pathways. Conclusion: AG inhibited 3T3-L1 preadipocyte differentiation to a certain extent, suggesting its potential to ameliorate lipid metabolism disorder. The results of lipidomics showed that AG could improve the abnormal state of lipid metabolism during adipocyte differentiation by regulating the levels of fatty acid and phospholipid metabolites.
  • Study on the effect of skin integrity on the permeability of rivastigmine transdermal patches*
    MA Xun, TANG Hong-min, FENG Rui-ni, LI Tian-yu, DING Qi, WANG Qing, YU Li-ju, CHEN Hua
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1360-1366. https://doi.org/10.16155/j.0254-1793.2024-1263
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To use rivastigmine transdermal patches as a model drug, to study the changes in trans-epidermal electrical resistance (TEER) and trans-epidermal water loss (TEWL) during in vitro permeation testing (IVPT), and to evaluate their correlation with the total cumulative amount (AMT) and permeation rate, so as to elucidate their relevance to drug permeation behavior. Methods: Skin samples with similar thickness and acceptable TEWL values but varying TEER levels (in multiples) were selected for the IVPT of rivastigmine transdermal patches. The stratum corneum was disrupted using the tape stripping method, and TEWL, TEER, and AMT were compared before and after stripping. Results: For skin with uniform thickness and acceptable TEWL (<15 g · m-2 · h-1), the AMT of rivastigmine patches showed a linear correlation with time (t1/2), with a correlation coefficient r>0.99. Additionally, the TEER multiple was linearly correlated with the permeation rate (r>0.99). In skin with compromised barrier integrity (damaged stratum corneum), TEWL increased by approximately 2-3 times, while the TEER decreased by about 10-fold, and the AMT significantly increased. Conclusion: TEER multiples exhibited a linear correlation with the permeation rate of the rivastigmine transdermal patch. Both TEWL and TEER multiples can be used to assess skin integrity, with preliminary results suggesting that the TEER method has higher sensitivity.
    • Safety Monitoring
  • Analysis of microbiological contamination of prepared slices of baked licorice based on mass spectrometry
    TANG Rong, TENG Yun, ZHANG Min-juan
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1367-1379. https://doi.org/10.16155/j.0254-1793.2024-1112
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To investigate the microbial contamination of 74 batches of prepared slices of baked licorice and to provide the reference for microbial limit test and criteria of baked licorice. Methods: Referring to the methods in chapters 1105, 1106 and 1108 of the Pharmacopoeia of the People's Republic of China (the Chinese Pharmacopoeia) 2020 edition, 74 batches of samples were examined for total aerobic bacteria (TAMC), total molds and yeasts (TYMC) and total heat-resistant bacteria (HRMC). And the three types of control bacteria, and the typical colonies were identified by using MALDI-TOF-MS, to preliminarily reaveal the level of bioburden of prepared slices of baked licorices and analyze the microbial contamination. Results: The lg values of TAMC in 74 batches of prepared slices of baked licorice ranged from 1.7 to 6.7, with a mean value of 3.6, the lg values of TYMC ranged from 0 to 5.9, with a mean value of 2.3, and the lg values of HRMC ranged from 0 to 6.0, with a mean value of 2.7. Contamination with bile salt resistant gram-negative bacteria was uneven, 43 batches were detected with bile salt resistant gram-negative bacteria. Escherichia coli and Salmonella were not detected in 74 batches, and a total of 18 genera and 44 species of other bacteria were detected. Conclusion: The microbial contamination of prepared slices of baked licorice varies widely and is uncertain, and there is a risk of microbial contamination in production, circulation and use, which is affected by planting and harvesting, preparation process, storage environment and transportation conditions, etc. The pathogenic bacteria detected suggests that the contaminated microorganisms in prepared slices of baked licorice have a certain degree of pathogenicity, and effective measures should be taken to prevent microbial contamination and to establish a reasonable microbial quality standard to improve the quality of prepared slices of baked licorice.
  • Study on the detection of osmium in ointment preparations
    SUN Yi-shu, CUI Yin-xin, ZHANG Ye, YE Xiao-xia, LE Jian
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1380-1384. https://doi.org/10.16155/j.0254-1793.2025-0042
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To develop a method based on microwave digestion followed by inductively coupled plasma mass spectrometry (ICP-MS) for the determination of osmium in ointment preparations. Methods: Accurately weighed 0.1 g of each sample and added 5 mL of nitric acid. The samples were digested using microwave-assisted digestion. After cooling, 10 mL of a 50 g · L-1 thiourea solution was added. The mixture was then heated in a sealed vessel at 100 ℃ for 1 h. Osmium content was sebsequently determined by ICP-MS. Results: Good linearity (r>0.999) was demonstrated over the concentration range of 6 to 40 μg · L-1. Recovery rates at three spiking levels (30%, 100%, 150%) for three types of ointment ranged from 76.5% to 112.0%. Osmium was not detected in any of the six batches tested across the three ointment formulations. Conclusion: The developed method demonstrates good linearity, high sensitivity, satisfactory accuracy, and excellent precision. It is suitable for the determination of osmium in ointment-based pharmaceutical products.
  • GC-MS detection of extractable amounts of different types of plasticizers in pharmaceutical packaging materials
    ZHANG Feng-lan, REN Jing, ZHENG Ye
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1385-1392. https://doi.org/10.16155/j.0254-1793.2025-0013
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To establish a GC-MS method for simultaneous determination of extractable amounts of 21 plasticizers from 4 common types (phthalates, citrate esters, terephthalates, polyester) in pharmaceutical packaging materials. Methods: Plasticizers in the pharmaceutical packaging material samples were extracted using n-hexane by ultrasound at 40 ℃ for 30 min. The extract was filtered through a 0.22 µm organic membrane filter, separated on a Select PAH capillary chromatography column, qualitatively analyzed by GC-MS in full scan mode, and quantitatively analyzed in selected ion monitoring mode. Results: All 21 plasticizers were completely separated within 35 min. In the concentration range of 0.02 to 2 µg · mL-1, good linearity was observed between concentration and peak area, with correlation coefficients all above 0.994. The detection limits for all target compounds were less than 0.01 µg · mL-1. The recoveries of spiked samples ranged from 87.8% to 118.0%. The method was applied to 14 batches of pharmaceutical packaging materials (plastic bottles, rubber stoppers, infusion bags), and plasticizers were detected in 6 batches, including diisobutyl phthalate (DIBP), di-n-butyl phthalate (DBP), bis (2-ethylhexyl) phthalate (DEHP), and acetyl tributyl citrate (ATBC). Conclusion: The method established in this study for the simultaneous determination of extractable amount of 21 plasticizers of different types has high sensitivity and good repeatability, and is suitable for rapid determination of plasticizers in pharmaceutical packaging materials.
    • Rapid Analysis
  • Rapid authentication of Bungarus Parvus by loop-mediated isothermal amplification*
    WANG Xi, ZHANG Jin-ju, ZHONG Wen-ting, MA Zhi-guo, WU Meng-hua, CAO Hui, ZHANG Ying
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1393-1398. https://doi.org/10.16155/j.0254-1793.2024-1306
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To develop a rapid and visual identification method for Bungarus Parvus, a well-known traditional Chinese medicine, using loop-mediated isothermal amplification (LAMP). Methods: Two pairs of primers (outer primer YHS-F3, YHS-B3 and inner primer YHS-FIP, YHS-BIP) were designed based on specific loci of the cytochrome b(cyt B) gene of Bungarus Parvus. The LAMP reaction system, comprising template DNA, primers, Bst DNA polymerase and SYBR Green Ⅰ fluorescent dye, was amplified at 60 ℃ for 60 min. The LAMP results were visually assessed by color change and compared with DNA barcoding and polymerase chain reaction (PCR) to evaluate specificity and sensitivity. Results: All 10 batches of Bungarus Parvus samples tested positive, with the reaction solution changing from orange to green. In contrast, other snake species remained orange after the reaction. The LAMP results were in complete agreement with those obtained from DNA barcoding and PCR. The detection limit of the LAMP method was 1×10-6 μg · mL-1. Conclusion: The established LAMP method is accurate, sensitive and easy to operate. It requires minimal equipment and can be applied for the rapid screening and authentication of Bungarus Parvus.
  • Three-dimensional fluorescence rapid detection technology in the exploratory research of drug supervision and sampling inspection Ⅰ—Identification of authenticity and quality of traditional Chinese medicinal materials
    LI Hui-bo, SHI Cui-yi, WANG Tong, FAN Ying-ying, QI Xiao-ling, SU Jian, WANG Hao, XU Ji-jun, WU Hai-long, TIAN Run-tao
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1399-1412. https://doi.org/10.16155/j.0254-1793.2025-0050
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To explore the rapid inspection application of three-dimensional fluorescence technology in national drug sampling inspections, organize and construct an innovative technical system integrating high-dimensional spectroscopy and chemometric intelligent modeling, and apply it in quality evaluation of traditional Chinese medicine. Methods: Three-dimensional fluorescence fingerprint spectra of 131 batches of samples, including six traditional Chinese medicines (Aquilariae Lignum Resinatum, Olibanum, Angelicae Dahuricae Radix, Persicae Semen, Stephaniae Tetrandrae Radix and Faeces Trogopterori) and their common adulteration from annual national drug sampling were collected using a three-dimensional fluorescence spectrometer. The Rayleigh scattering and Roman scattering were removes using a piecewise Hermite spline interpolation algorithm. The spectra were factorized by the self-weighting alternating trilinear decomposition (SWATLD) algorithm. Establish three-dimensional fluorescence spectral qualitative models for Aquilariae Lignum Resinatum versus its counterfeit Syringa Pinnatifolia, Olibanum versus its counterfeit Succlnum, Angelicae Dahuricae Radix versus sulfur-fumigated Angelicae Dahuricae Radix, Persicae Semen versus Armeniacae Semen Amarum, Stephaniae Tetrandrae Radix and its counterfeits, as well as Faeces Trogopterori versus artificial Faeces Trogopterori, etc., using various chemometric algorithms such as principal components analysis (PCA), hiearchical cluster analysis (HCA), partial least squares discriminant analysis (PLS-DA), and these models were applied to the rapid inspection and identification of the authenticity, quality, and inferiority of traditional Chinese medicines. Finally, cross-validation was used to evaluate the specificity and sensitivity of the models. Results: The modeling technology based on three-dimensional fluorescence spectra could achieve direct, rapid, green, and near-real-time intelligent qualitative analysis of the quality of traditional Chinese medicines. The correct recognition rate of each model reached 100%. Conclusion: Different traditional Chinese medicines have characteristic three-dimensional fluorescence fingerprint information. The chemometric models established by three-dimensional fluorescence spectra and the SWATLD factor decomposition algorithm can effectively characterize and evaluate the quality differences between traditional Chinese medicines and their common adulteration.
    • Quality Control
  • Characterization of the component profile and degradation products of polysorbate 80 by UHPLC-Q TOF/MS*
    WANG Dan, MA Cong-yu, ZHAO Xun, HUANG Qing, SHI Hai-wei
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1413-1426. https://doi.org/10.16155/j.0254-1793.2025-0054
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To comprehensively characterize the component profile of polysorbate 80 (PS80) using ultra high performance liquid chromatography-quadrupole time-of-flight/mass spectrometry (UHPLC-Q TOF/MS), to identify its degradation products, to investigate the effects of different buffer systems (citrate, phosphate, and histidine buffers), acid-base hydrolysis, and oxidative degradation on the PS80 component profile, to identify new degradation products of PS80 and its degradation behavior and potential mechanisms under various stress conditions. Methods: PS80 and its stress samples (subjected to acid-base hydrolysis or Fe2+-induced oxidative degradation in citrate, phosphate, and histidine buffer systems) were separated using an Agilent ZORBAX RRHD SB-C8 column (100 mm×2.1 mm, 1.8 μm) with gradient elution employing 0.1% formic acid in water and 0.1% formic acid in acetonitrile as the mobile phase. Mass spectrometric analysis was performed in positive electrospray ionization (ESI+) mode with full-scan MS (m/z 100-3 000) and MS/MS under collision energies of 80 eV (for doubly charged ions) and 120 eV (for singly charged ions). Molecular ions, fragment ions, and degradation patterns of PS80 components were analyzed to deduce the structures of degradation products and elucidate potential degradation pathways. Results: Nine major components of PS80 were successfully separated and identified using UHPLC-Q TOF/MS. PS80 exhibited greater stability under acidic conditions compared to alkaline conditions. In histidine buffer, Fe2+ readily induced oxidative degradation of unsaturated esters in PS80, generating four representative oxidative degradation products: polyoxyethylene iso-sorbitol 9-oxononanoate monoester, polyoxyethylene iso-sorbitol epoxy stearate monoester, polyoxyethylene sorbitan ketostearate monoester, and polyoxyethylene ketostearate monoester. Conclusion: The UHPLC-Q TOF/MS technique is effectively utilized to comprehensively identify and characterize the component profile of PS80. The findings enhance the understanding of PS80 behavior in complex pharmaceutical systems and provide valuble insights for pharmaceutical formulation design.
  • Study on the classification and nomenclature changes of strains in live microecological products based on average nucleotide identity (ANI) across the whole genome
    FENG Dan-yang, HU Wen-hong, GUO Jun-zhen, XING Sheng, DING Bo
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1427-1441. https://doi.org/10.16155/j.0254-1793.2024-1232
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To confirm the species information of strains in live microecological products using whole-genome sequence data and average nucleotide identity (ANI) analysis, thereby clarifying their classification and nomenclature. Method: Strains from commercially available live microecological products were isolated and purified. Sixteen strains underwent high-throughput sequencing, and the resulting whole-genome sequences were compared with authenticated reference genomes in the NCBI database using FastANI software. The species information of the strains was ascertained based on the ANI analysis results. Results: The results showed that the 16 strains belonged to 11 different species, of which 6 species exhibited nomenclature inconsistencies with their original designations, affecting more than half of the live microecological products on the market. Conclusion: It is recommended to correct some wrongly named strain names according to the actual species information, establish a strain genetic information database for the production of microecological live bacteria products. Regular genetic information verification and comparison of these strains should be conducted to ensure the safety and quality of live microecological products.
  • Quality evaluation of Farfarae Flos from different habitats based on the method of QAMS combined with chemical pattern recognition, weighted TOPSIS and grey relational analysis fusion model
    SONG Yi, WANG Quan
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1442-1457. https://doi.org/10.16155/j.0254-1793.2025-0041
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To establish a method for evaluating quality difference of Farfarae Flos from different habitats by quantitative analysis of multicomponents by single marker (QAMS) method combined with chemical pattern recognition, and weighted technique for order preference by similarity to an ideal solution (TOPSIS) and grey relational analysis (GRA) fusion model, and to improve the quality control level. Methods: High performance liquid chromatography (HPLC) was applied with a gradient elution of acetonitrile (A) and 0.1% phosphoric acid aqueous solution (B) as the mobile phase. The detection wavelengths were 256 nm (adenosine, rutin, and isoquercitrin), 326 nm (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, isochlorogenic acid B, isochlorogenic acid A, and isochlorogenic acid C), and 220 nm (tussilagone). The flow rate was 1.0 mL · min-1 and the column temperature was 30 ℃. The contents of adenosine, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, rutin, isoquercitrin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C and tussilagone in 19 batches of Farfarae Flos were determined by QAMS using isochlorogenic acid B as the internal reference substance. The extracts were determined according to Chinese Pharmacopoeia (2020 edition). Chemical pattern recognition was used to analyze the quality differences of samples from different habitats and reveal the characteristic components that caused the quality differences. The quality of 19 batches of Farfarae Flos was ranked, and the quality difference of Farfarae Flos from different habitats was evaluated by weighted TOPSIS and GRA fusion model. Results: There was no significant difference between the results determined by QAMS and external standard method (ESM). The contents of adenosine, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, rutin, isoquercitrin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C and tussilagone in 19 batches of Farfarae Flos were 0.106%-0.192%, 0.021%-0.061%, 0.622%-1.247%, 0.041%-0.103%, 0.004%-0.017%, 0.069%-0.248%, 0.027%-0.075%, 0.596%-1.443%, 0.504%-0.968%, 0.314%-0.781% and 0.045%-0.109%, respectively. Through chemical pattern recognition, 19 batches of samples were grouped into 3 categories, and the characteristic components affecting the quality of Farfarae Flos were chlorogenic acid, isochlorogenic acid A, tussilagone and isoquercitrin. In the weighted TOPSIS and GRA fusion model, the relative closeness of 19 batches of samples was 0.221 1-0.761 8, and there were quality differences in the Farfarae Flos samples from different habitats. The quality ranking from best to worst was: samples from Gansu, Shanxi, Hebei, Henan and Neimenggu. Conclusion: The established method of QAMS combined with chemical pattern recognition, and weighted TOPSIS and GRA fusion model can evaluate the quality of Farfarae Flos comprehensively and objectively, and the method provides a basis for the quality control and regional difference research.
    • Standard Deliberation
  • Clarification and application considerations for the terms “Specificity” and “Selectivity” in analytical procedures*
    GENG Ying, ZHU Rong-die, YUE Rui-qi, WU Yan-lin, CHEN Hua, LIU Yi, TAN De-jiang, SUN Hui-min
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(8): 1458-1464. https://doi.org/10.16155/j.0254-1793.2024-1117
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    This article traces and compares the origins, distinctions, and interrelationship of the two terms—specificity and selectivity—as used in pharmaceutical analytical methods. It discusses how these terms have been harmonized and incorporated into the guidelines of the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH). The article also introduces the approaches for evaluating and applying these terms in analytical procedures. Finally, case examples are provided to further illustrate their practical implications and to enhance readers' understanding of the concepts.
京ICP备17052540号-4
Copyright © Chinese Journal of Pharmaceutical Analysis, All Rights Reserved.
E-mail：ywfx@nifdc.org.cn
Powered by Beijing Magtech Co. Ltd.