31 March 2026, Volume 46 Issue 3
    

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    Special Column on Quality Analysis and Research of Proprietary Chinese Medicines in National Drug Sampling and Testing
  • Method research of the anti-atherosclerosis mechanism and quality evaluation of Naoluotong capsules based on network pharmacology*
    ZHOU Ying, WANG Rong, LU Jing-xian, ZHENG Cheng, XU Zhe, DUAN Ming-yang, YAO Yao, CHEN Bi-lian
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 379-393. https://doi.org/10.16155/j.0254-1793.2025-0333
    Abstract ( )   Knowledge map   Save
    Objective: To investigate the anti-atherosclerosis mechanism and improve the quality control standards of Naoluotong capsules. Methods: The anti-atherosclerosis mechanism of Naoluotong capsules was explored by integrating network pharmacology and cell experiments. On the basis of key pharmacodynamical compounds, a high-performance liquid chromatography (HPLC) method was established to determine the content of salvianolic acid B, tolperisone hydrochloride, methyl hesperidin, and vitamin B6. Results: Network pharmacology, molecular docking, and cell experiments confirmed that salvianolic acid B and tolperisone hydrochloride in Naoluotong capsules significantly inhibited macrophage foam cell formation. The developed HPLC method demonstrated excellent linearity for the four components (r≥0.999 8), with recovery rates ranging from 99.3% to 102.1% (relative standard deviation≤2.6%). In 53 batches of samples, the content of salvianolic acid B, tolperisone hydrochloride, methyl hesperidin, and vitamin B6 varied within the ranges of 0.001-1.92 mg per capsule, 35-54 mg per capsule, 3.8-11.0 mg per capsule, and 1.0-2.3 mg per capsule, respectively. Conclusion: Naoluotong capsules exert anti-atherosclerosis effects by multi-target regulation of inflammatory and lipid metabolism pathways. The established activity-guided multi-component quality control method for the in vitro model enables precise quantification of key bioactive components, providing a scientific basis for enhancing the quality standards and ensuring consistency in clinical efficacy of this compound formulation.
  • Quality evaluation of Siji Ganmao preparations based on national drug evaluation sampling and testing*
    ZHENG Wen-yan, LI Pan-lin, JIAN Shu-yi, LIAN Xiao-yin, ZHU Hui-ru, LIU Jing, LIU Xiao-xiao
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 394-407. https://doi.org/10.16155/j.0254-1793.2025-0387
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    Objective: To systematically evaluate the quality of Siji Ganmao preparations based on the national drug evaluation sampling, analyze the existing quality problems, and provide references and suggestions for improving the quality control. Methods: A total of 193 batches of samples were tested according to the statutory standards. According to the prescription, production technology, and current quality standards, exploratory research was carried out around the material bases, production process, quality control, and consistency and safety of drugs, for comprehensively assessing the quality of Siji Ganmao preparations. Results: The qualified rate for 193 batches of samples was 100%. A multi-component thin-layer chromatography identification method, characteristic fingerprint of volatile components, and multi-indicator component content determination method were established and can be applied to the quality control and evaluation of Siji Ganmao preparations. The exploratory research showed that some batches of samples had problems such as the quality of raw medicinal materials used in production and the stability of production processes, which required improvement. Conclusion: It is recommended that manufacturers of Siji Ganmao preparations strengthen the control over the sources of drugs and production processes. Since the current quality standards cannot effectively guarantee the quality of preparations, revision and improvement of the quality standards are needed.
  • Quality analysis of Chinese patent medicines based on 2023—2024 national drug sampling and testing*
    LIU Jing, HE Feng-yan, ZHOU Ya-nan, CHENG Xian-long, WANG Chong, WEI Feng
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 408-414. https://doi.org/10.16155/j.0254-1793.2025-0490
    Abstract ( )   Knowledge map   Save
    National drug sampling and inspection is an important measure for post-market drug supervision in China. It serves as crucial technical support for implementing risk management and pre-supervision. Over the past two decades, it has played an irreplaceable role in actively ensuring drug quality and safety, particularly in cracking down on adulteration and counterfeiting, eliminating quality hazards, and elevating quality control standards. From 2023 to 2024, the national drug sampling and inspection involved a total of 91 varieties of Chinese patent medicines. The work adopted a comprehensive evaluation mode of standard testing combined with exploratory research. And systematic and in-depth research on the material input, safety, effectiveness, and quality consistency of the tested varieties has been conducted under the guidance of the principles of problem orientation and risk prevention and control. This article evaluated the overall quality status of Chinese patent medicines in China over the past two years based on the quality analysis reports and sorted out and summarized the common quality issues found in each variety. It provides an effective reference and basis for building a more scientific, efficient, and authoritative post-market supervision system for drugs, improving the scientificity, targeting, and accuracy of drug sampling and inspection, and enhancing the practical effectiveness of serving traditional Chinese medicine supervision.
  • Quality analysis of proprietary Chinese medicines containing ginseng (red ginseng) based on 2021—2024 national drug sampling and testing*
    HE Feng-yan, GUO Ri-xin, ZHOU Ya-nan, WANG Ya-nan, LIU Jing, WEI Feng
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 415-423. https://doi.org/10.16155/j.0254-1793.2025-0494
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    National drug sampling and inspection is an important means of post-marketing drug supervision. From 2021 to 2024, 16 varieties of Chinese patent medicines containing ginseng (red ginseng) such as Shengui Lurong pills and Shenling Baizhu preparations were sampled and inspected nationwide, with a total of 1 740 batches of samples. The data of 16 varieties were systematically reviewed and analyzed. The main quality problems of these varieties were summarized. The common quality problems of ginseng (red ginseng)-containing Chinese patent medicines were identified. Recommendations for supervision and quality improvement of ginseng (red ginseng)-containing Chinese patent medicines were proposed.
  • Simultaneous determination of six components in Shujin Dingtong tablets by UPLC-MS/MS*
    ZHOU Ya-nan, HU Xiao-ru, DAI Zhong, WEI Feng, LIU Jing
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 424-430. https://doi.org/10.16155/j.0254-1793.2025-0497
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    Objective: To establish an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for simultaneous determination of syringin, 6-hydroxykaempferol 3,6-diglucoside, kaempferol 3-O-β-D-glucuronide, naringin, aloe-emodin, and senkyunolide A in Shujin Dingtong tablets and comprehensive evaluation of the quality of Shujin Dingtong tablets. Methods: An ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm) was used for gradient elution with acetonitrile as mobile phase A and 0.1% formic acid aqueous solution as mobile phase B. Multiple reaction monitoring (MRM) was adopted for scanning under positive and negative ion modes. Results: All the components showed good linear relationships between peak areas and concentrations within their tested ranges. The recovery rate met the requirements of each concentration level. The content of syringin, 6-hydroxykaempferol 3,6-diglucoside, kaempferol 3-O-β-D-glucuronide, naringin, aloe-emodin, and senkyunolide A in Shujin Dingtong tablets was 0-8.47 µg, 0-10.80 µg, 0-2.52 µg, 26.38-220.65 µg, 10.80-116.88 µg, and 5.45-177.60 µg per tablet, respectively. Conclusion: The six components in Shujin Dingtong tablets are from Carthami Flos, Drynariae Rhizoma, Rhei Radix et Rhizoma, and Angelicae Sinensis Radix, respectively. The established method is simple, and accurate and can comprehensively evaluate the quality of Shujin Dingtong tablets.
    • Review & Monography
  • Comparative research progress in Chaxiong Rhizoma and Chuanxiong Rhizoma*
    SUN Xiao-li, QIU Zhi-yan, YANG Jian-bo, CHEN Shu, HU Sheng-mou, XIA Ming-yan, XU Cong-long, WANG Can-jian, ZHANG Guo-song
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 431-443. https://doi.org/10.16155/j.0254-1793.2025-0483
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    Chaxiong Rhizoma and Chuanxiong Rhizoma are both derived from plants of Ligusticum (Umbelliferae). Both of them have remarkable effects of promoting qi and blood circulation, expelling wind and relieving pain, and their application history can be traced back to ancient times. Chaxiong Rhizoma is a key component of many classic prescriptions, playing an important role in clinical practice. However, in the long development history of traditional Chinese medicine, Chuanxiong Rhizoma has occupied the mainstream position in the market, and the medicinal value of Chaxiong Rhizoma has not attracted due attention. By combing the literature records and comparative studies of Chuanxiong Rhizoma and Chaxiong Rhizoma at home and abroad, this paper performs a comprehensive analysis from six aspects: herbal textual research, growth environment, identification characteristics, chemical components, pharmacological effects, and functions, and probes into their similarities and differences, aiming at clarifying the historical status of Chaxiong Rhizoma and tap its medicinal potential. At the same time, basing on the background of modern research of traditional Chinese medicine, we make an outlook on the development prospects of Chaxiong Rhizoma and provide ideas for the rational development and comprehensive utilization of Chaxiong Rhizoma resources.
  • A literature review of electrochemical detection methods for arsenic concentration and valence state*
    DING Yi, LIU Jing-yu, ZHANG Yu-bi, ZHANG Yun-zheng, CHEN Wang, ZHANG Ke-xin, WANG Xian-shu, LI Ya-nan
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 444-453. https://doi.org/10.16155/j.0254-1793.2025-0375
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    Arsenic (As) is a highly toxic metal contaminant, and the precise detection of its various forms (especially the highly toxic As (Ⅲ) within the environment and living organisms play a crucial role in ecological security and precision medicine. While spectroscopy/mass spectrometry techniques offer high sensitivity, they are limited by high costs, operation complexity, and difficulties in differentiating valence states in the field. Electrochemical methods, with high sensitivity, rapid responses, low costs, and the potential for form resolution, have emerged as ideal alternatives. This paper systematically reviews the progress in electrochemical detection of inorganic arsenic. Specifically, gold/silver nanomaterials, through the micro-nano structures (such as rose petal template gold electrodes and plasma-deposited Ag/Au nanoplates), have significantly enhanced the detection performance; transition metal oxides (such as Fe-Co-LDH/MXene) and MOF/COF materials (such as Ti-MOF and BPTB-COF) have utilized synergetic effects and specific adsorption for ultra-trace detection; biomarking strategies (using biologically sourced active materials) provide novel ideas for complex matrix analysis. These technologies have been successfully applied to the quality control of water bodies and foods, and future studies need to further solve the issues of interferences from real sample matrices and to extend the standardized application of these technologies in the safety monitoring of Chinese medicinal materials such as Realgar.
    • Ingredient Analysis
  • Study on mineralogical characterization of Pyritum based on AMICS*
    WANG Cheng-cheng, LU Min, CHEN Jing-xu, LI Juan, ZHENG Guo-hua, CAO Yan
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 454-462. https://doi.org/10.16155/j.0254-1793.2024-1323
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    Objective: To obtain comprehensive mineralogical information, a systematic study was conducted on the Pyritum's surface properties, mineral composition, elemental composition, and occurrence state of iron element by means of the advanced mineral identification and characterization system (AMICS). Methods: Energy spectrum analyzer with scanning electron microscope, X-ray diffractometer, specific surface and pore size analyzer, and X-ray photoelectron spectrometer were used for the preliminary physical phase analysis of the Pyritum, and then the AMICS was employed for the comprehensive mineralogical characterization analysis of the Pyritum. Results: The dendritic Pyritum crystals from Yunnan Province exhibited a denser surface, presenting a distinct microscopic morphology compared to other samples. This origin's Pyritum also contained a higher overall proportion of Fe and S, compared with that of other origins, with Fe2+ accounting for a higher proportion. The AMICS results showed that the Pyritum phase included 18 minerals, with pyrite and magnetite as the predominant mineral species. Notably, 94.38% of the pyrite particles existed in a high-degree-of-freedom state. The weak symbiotic relationship between pyrite and other associated minerals made the associated minerals prone to separation. Beyond the predominant elements Fe, S, O, and Si, the Pyritum contained trace elements such as K, Mg, Ca, and Mn. Fe was primarily distributed in pyrite and magnetite, whereas S was found exclusively in pyrite and pyrrhotite. Conclusion: By combining AMICS technology for the first time, the mineralogical study of Pyritum can obtain rich mineralogical characterization information, laying a solid foundation for basic research on medicinal resources, quality evaluation, standard formulation, and concoction process of Pyritum.
  • Application of an electrochemical sensor in morphine detection*
    REN Shu-fang, CHEN Yu, CAO Li, LIU Ya-hui, WANG Zi-han, LIU Xiao-hang, LIU Di
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 463-473. https://doi.org/10.16155/j.0254-1793.2025-0328
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    Objective: To develop an electrochemical sensor for the quantitative detection of morphine. Methods: The metal-organic framework ZIF-67 and acidified multi-walled carbon nanotubes (MWCNTs) were used to synthesize the composite AZIF-67/MWCNTs. The composite was drop-cast onto a glassy carbon electrode (GCE) to fabricate a electrochemical sensor ZIF-67/MWCNTs/GCE, which enabled highly sensitive and selective detection of morphine. Results: ZIF-67/MWCNTs/GCE exhibited a favorable current response to morphine, with a linear detection range of 10-100 μmol · L-1 and a limit of detection (LOD) of 5.76 μmol · L-1 (S/N=3). Additionally, the modified electrode demonstrated excellent stability, repeatability, and anti-interference capabilities. Recovery rates for morphine spiked in real samples ranged from 93.6%-97.8%, with RSD<5% (n=3). Conclusion: The electrochemical sensor developed in this study offers high sensitivity and reliability for morphine detection. With low-cost raw materials and simple fabrication, it holds promising potential for practical applications in morphine detection.
    • Metabolism Analysis
  • Quantification of salbutamol, formoterol, and carboxy-THC in human urine by UPLC-HRMS for anti-doping analysis*
    LIU Lu, YAN Kuan, HE Gen-ye, DONG Tian-yu, ZHANG Yu-feng, MA Cong-cong, WANG Zhan-liang
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 474-483. https://doi.org/10.16155/j.0254-1793.2025-0451
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    Objective: To establish an accurate quantitative method for salbutamol, formoterol, and 11-nor-Δ9-tetrahydrocannabinol-carboxylic acid (carboxy-THC) in human urine based on ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). Methods: The quantitative bias caused by pretreatment operations and matrix effects was reduced by the dilute-and-shoot pretreatment method after hydrolysis with glucuronidase. A Parallel Reaction Monitoring (PRM) mode was employed for detection. Results: The method validation experiment showed an excellent linearity between 50% and 200% threshold concentrations, with the linear coefficient (r) ranging from 0.998 7 to 0.999 7. The relative standard deviation (RSD) at the limit of quantification were lower than 10.0%. The uncertainty (Uc) was below the maximum uncertainty specified in the technical document of the World Anti-Doping Agency (WADA). Conclusion: The method is characterized by operational simplicity and high accuracy and reliability of results. It has obtained certification from the China National Accreditation Service for Conformity Assessment (CNAS), and the analytical results obtained with this method have passed the WADA-external quality assessment schemes. This method has been applied in routine tests of doping detection and large-scale sports events such as the 2022 Beijing Winter Olympics.
    • Safety Monitoring
  • Methanesulfonate impurity determination and quality evaluation of dabigatran etexilate capsules and dabigatran etexilate mesylate based on GC-MS/MS*
    XU Yue-ting, GENG Xiao-ting, LIU Yan-shu-xian, CHEN Ping-ping, AI Jie, XIE Sheng-gu, GU Xiao, SHAO Peng
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 484-492. https://doi.org/10.16155/j.0254-1793.2025-0229
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    Objective: To establish a gas chromatography-tandem mass spectrometry (GC-MS/MS) method for the determination of methanesulfonate impurities in dabigatran etexilate capsules and dabigatran etexilate mesylate, and to evaluate the product quality. Methods: Samples were concentrated by multi-step liquid-liquid extraction. The analytes were separated through a DB-624 quartz capillary column (30 m×0.32 mm, 1.8 μm), with an inlet temperature of 230 ℃, a carrier gas flow rate of 1.5 mL · min-1, and an injection volume of 2 μL. The analysis was performed according to the set program heating conditions. Detection was carried out with electron impact (EI) ion source in the multi-reaction monitoring (MRM) mode. Propyl methanesulfonate (PMS) and butyl methanesulfonate (BMS) were used as internal standards for the determination of methyl methanesulfonate (MMS), ethyl methanesulfonate (EMS), isopropyl methanesulfonate (IMS), and hexyl methanesulfonate (HMS). Results: The four methanesulfonate impurities showed good linearity (r>0.995 0) between peak area and concentration in their respective concentration ranges. The limits of detection (LODs) were 0.301-2.01 ng · mL-1 and the limits of quantification (LOQs) were 0.606-4.02 ng · mL-1. The average recovery rates of impurities were between 86.8% and 113%, with the RSD<3% (n=3). The 18 batches of capsule samples and 4 batches of API samples showed the HMS content of 0.118-0.527 μg · g-1 and the content of other three impurities lower than LOQs. The content of four methanesulfonate impurities was all lower than 5 μg · g-1. Conclusion: This method is specific, accurate, and sensitive and thus can be used for simultaneous determination of methanesulfonate impurities in dabigatran etexilate capsules and dabigatran etexilate mesylate to provide reference for improving the national standard of dabigatran etexilate capsules and experimental support for quality control of products.
  • Effects of two processing excipients on the chemical composition of Aconiti Lateralis Radix Praeparata based on UHPLC-Q Exactive Focus MS/MS*
    LI Sha-sha, LIU Ya-feng, WANG Wei-feng, LI Fang, LI Fan, MAO A-juan, LIU Man-jun, ZHANG Cai-ping
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 493-504. https://doi.org/10.16155/j.0254-1793.2025-0270
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    Objective: To rapidly analyze and identify the alkaloids in Aconiti Lateralis Radix Praeparata and two types of processed products using ultra-high-performance liquid chromatography-quadrupole-electrostatic field orbital trap high resolution mass spectrometry (UHPLC-Q Exactive Focus MS/MS), and to evaluate the scientific validity of processing Aconiti Lateralis Radix Praeparata with calcium chloride. Methods: A Waters Acquity UPLC BEH C18 column (2.1 mm×50 mm, 1.7 μm) was employed, with gradient elution performed using a mobile phase consisting of acetonitrile and 0.1% formic acid aqueous solution. The electrospray ion source (ESI) was adopted to collect the data in positive ionization mode within a mass-to-charge (m/z) range of 100-1 500. Chemical components were identified by integrating mass spectrometry data, including relative molecular mass and fragment ions, with reference substances, databases, and relevant literature. Principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA) and variable importance projection (VIP) were used to pinpoint the differential components of Aconiti Lateralis Radix Praeparata and two types of products processed with brine and calcium chloride, respectively. The ion peak area ratio of each component before and after processing was used as the index for the variation in comparative analysis. Results: A total of 187 common compounds were identified in Aconiti Lateralis Radix Praeparata, with 36 potential differential chemical components preliminarily confirmed. Conclusion: The two processing excipients have the same influencing trends on the chemical components of Aconiti Lateralis Radix Praeparata, confirming the feasibility of processing Aconiti Lateralis Radix Praeparata with calcium chloride. This provides experimental basis and data support for clarifying the scientific connotation of calcium chloride-based processing of Aconiti Lateralis Radix Praeparata.
  • Structural identification of related substances of fulvestrant by chromatography-mass spectrometry*
    ZHAO Qi-qian, ZHENG Guo-gang, SHAO Peng, XU Yue-ting, CHEN Ping-ping, GU Xiao, WU Yi-hang
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 505-516. https://doi.org/10.16155/j.0254-1793.2025-0199
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    Objective: To identify the related substances of fulvestrant by ultra high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UHPLC-Q TOF/MS) for its production process optimization and quality research. Methods: An Eclipse XDB-C18 column (2.1 mm×100 mm, 1.8 μm) was used for separation of the related substances via gradient elution with methanol-acetonitrile-water as the mobile phase at a detection wavelength of 225 nm and a column temperature of 45 ℃. An electrospray ionization (ESI) source was employed to collect primary and secondary mass spectrometry data. The accurate mass and elemental composition of each related substance were determined, and the ion structures of the substances were identified. Results: Under the established chromatographic and mass spectrometric conditions, fulvestrant and its related substances were effectively separated. A total of nine major related substances were detected, and five of them had not been reported. Conclusion: Chromatography-mass spectrometry technology can effectively separate and identify the related substances of fulvestrant, providing reference for the production process optimization and quality research of fulvestrant.
  • Determination of related substances in loperamide hydrochloride by HPLC
    LIN Kai-wen, WU Hang, CHEN Nian-gen
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 517-526. https://doi.org/10.16155/j.0254-1793.2025-0337
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    Objective: To establish an HPLC method for the determination of related substances in loperamide hydrochloride. Methods: An Xtimate C18 column (4.6 mm×250 mm, 5 μm) was used for gradient dlution with a mobile phase consisting of 0.1% phosphoric acid solution and acetonitrile at the flow rate of 1.0 mL · min-1, the column temperature maintained at 35 ℃, the detection wavelength set at 220 nm and the injection volume of 20 μL. Results: The chromatographic peaks between loperamide hydrochloride and impurity Ⅰ, impurity Ⅱ, impurity Ⅲ, impurity Ⅳ, impurity Ⅴ, impurity Ⅵ, impurity Ⅶ, impurity Ⅷ, impurity Ⅸ, impurity Ⅹ, impurity Ⅺ, impurity Ⅻ, impurity ⅩⅢ, and impurity ⅩⅣ were well resolved. The resolution between all known impurities was≥1.5, and the method demonstrated good linearity (r>0.999 5, n=7) within the concentration range from the limit of quantitation (LOQ) to 200% of the specification limit. The correlation coefficients of loperamide hydrochloride and the known impurities all fell within the range of 0.999 6-1.000. The average recovery rates (n=9) fell within the range of 90.1%-104.5%. The limits of detection were 0.04-0.31 μg · mL-1, and the LOQs were 0.07-0.61 μg · mL-1. The content of relevant substances in three batches of loperamide hydrochloride was determined. The maximum content of a single impurity was 0.18%, and that of total impurities was no more than 0.3%. Conclusion: The developed method is accurate, sensitive, and reliable, thus being suitable for the determination of related substances in loperamide hydrochloride.
    • Quality Control
  • Quality evaluation of Glycyrrhiza uralensis Fisch. based on multi-component quantification and HPLC fingerprint*
    XU Xiao-qiong, MA Yu-quan, LI Xi-can
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 527-535. https://doi.org/10.16155/j.0254-1793.2025-0334
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    Objective: The HPLC fingerprint spectrum of Glycyrrhiza uralensis Fisch. was established, and the quality of Glycyrrhiza uralensis Fisch. was evaluated in combination with the chemometrics methods. Methods: The ZORBAX Eclipse Plus C18 (250 mm×4.6 mm, 5 μm) chromatographic column was adopted, using acetonitrile -0.1% phosphoric acid aqueous solution as the mobile phase, gradient elution was carried out at a flow rate of 1.0 mL · min-1, the detection wavelength was 237 nm, the column temperature was 30 ℃, and the injection volume was 20 μL. Results: In this study, a method for the simultaneous and rapid determination of the contents of seven index components in Glycyrrhiza uralensis Fisch. by HPLC was established. The precision, stability, repeatability and sample recovery experiments of this method all met the requirements. The consistency of the 10 batches of Glycyrrhiza uralensis Fisch. samples were good, and the similarity of the fingerprint spectra ranged from 0.946 to 0.992. The content of glycyrrhizic acid was the highest, liquiritigenin was the lowest, liquiritigenin fluctuated greatly, and isoliquiritin apioside was stable in Glycyrrhiza uralensis Fisch. samples. The quality of Glycyrrhiza uralensis Fisch. in Dengkou County, Bayannur City, Inner Mongolia was the best. Conclusion: HPLC fingerprinting combined with chemometrics methods can comprehensively and truly reflect the quality of Glycyrrhiza uralensis Fisch. and can be used for the quality evaluation of which. The research results have important guiding significance and reference value for the in-depth development of Glycyrrhiza uralensis Fisch. resources and the safe clinical medication.
  • Quality evaluation of compound Jiegeng Zhike tablets based on HPLC-CAD fingerprint combined with chemometrics and multi-component content determination*
    QIAN Ye-fei, ZHANG Chao, HUANG Yi-wen, WANG Ming-zhi, LU Lin-ling
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 536-549. https://doi.org/10.16155/j.0254-1793.2025-0318
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    Objective: To establish a fingerprinting and multi-component quantitative analysis method for compound Jiegeng Zhike tablets by high performance liquid chromatography coupled with a charged aerosol detector (HPLC-CAD), and comprehensively evaluate the quality differences of 31 batches of compound Jiegeng Zhike tablets from different manufacturers through chemometric approaches. Methods: Chromatographic conditions included an Agilent Zorbax Eclipse XDB C18 column (250 mm×4.6 mm, 5 μm), gradient elution with acetonitrile and 0.1% formic acid aqueous solution (flow rate: 1.0 mL · min-1, column temperature: 35 ℃, CAD power function value of 1.1, and injection volume of 10 μL. The fingerprint analysis identified 28 common peaks, with 12 components (e.g., platycodin E, platycodin D3, and polygalaxanthone Ⅲ) confirmed by comparison with reference standards. A quantitative method was further developed to assess quality variations among manufacturers. Results: Thirty batches (excluding 1 batch) of samples exhibited similarity above 0.90, indicating the reliability of the established fingerprint for holistic quality control of compound Jiegeng Zhike tablets. Chemometric analyses (hierarchical cluster analysis, principal component analysis, and orthogonal partial least squares-discriminant analysis) classified the 31 batches into six clusters and identified 15 potential discriminatory components. Quantitative analysis of the 31 batches revealed that the mass fractions of Platycodonis Radix-related components (platycodin E, platycodin D3, and platycodin D), Polygalae Radix-related components (polygalaxanthone Ⅲ, 3,6'-disinapoyl sucrose, tenuifolin, and onjisaponin B), Farfarae Flos-related components (isochlorogenic acid B, isochlorogenic acid A, and isochlorogenic acid C), and Glycyrrhizae Radix et Rhizoma-related components (liquiritin and glycyrrhizic acid) were 0.949-2.546 mg · g-1, 0.942-2.128 mg · g-1, 0.128-0.810 mg · g-1, and 0.240-0.744 mg · g-1, respectively. Conclusion: The proposed method achieves simple and accurate quality control of compound Jiegeng Zhike tablets based on HPLC-CAD fingerprint and multi-component content determination and systematically elucidates the material basis for the quality variations in compound Jiegeng Zhike tablets, laying a scientific foundation for enhancing quality standards and optimizing production processes.
  • Study on degradation of gluconate acid radical in zinc gluconate oral solution
    DENG Si-wei, SHAO Ran-wei, JIN Xin, ZHANG Ling, DAI Zhen
    Chinese Journal of Pharmaceutical Analysis. 2026, 46(3): 550-557. https://doi.org/10.16155/j.0254-1793.2025-0108
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    Objective: To study the molecular structure and production path of gluconate acid radical degradation products in zinc gluconate oral solution, aiming to provide a theoretical foundation for optimizing drug prescriptions and production processes. Methods: The compatibility between the raw material zinc gluconate and the excipient citric acid was investigated. The degradation product was obtained by designing degradation test, and the content of the degradation product was determined by the HPLC-CAD method. A Waters Xbridge BEH Amide chromatographic column (4.6 mm×150 mm, 5 μm) was employed, the mobile phase A was formate buffer (20 mmol · L-1 ammonium formate solution, with the pH adjusted to 3.0 using formic acid), and the mobile phase B was acetonitrile, gradient elution, the flow rate was 0.8 mL · min-1, the column temperature was maintained at 30 ℃, an electrospray detector was used, and the injection volume was 10 μL. Results: The results of the raw material-excipient compatibility test and degradation product content determination showed that gluconate radical degraded under acidic conditions, with degradation rates accelerated by heating. The identified degradation product was gluconolactone. Under the chromatographic conditions of this study, the linear range of the sum of D-glucose-δ-lactone and D-glucose-γ-lactone was 10.98-439.0 μg · mL-1 (r=0.997 1); the detection limits of D-glucose-δ-lactone and D-glucose-γ-lactone are 1.1 μg · mL-1 and 1.1 μg · mL-1 respectively, and the quantification limits are 2.7 μg · mL-1 and 2.8 μg · mL-1 respectively; the average recoveries of the sum of D-glucose-δ-lactone and D-glucose-γ-lactone at three concentration levels are 97.9%-100.8% (RSD=2.8%-3.9%, n=3). Conclusion: Under the existing prescription and production processes employed by various manufacturers for zinc gluconate oral solutions, the gluconate acid radical of zinc gluconate undergoes degradation to produce gluconolactone. This study serves as a reference for manufacturers to optimize prescriptions and production processes, while offering an experimental basis for improving the quality standards of this product.
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