31 May 2025, Volume 45 Issue 5
    

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    Review & Monography
  • Progress of online pretreatment technology in the application of biological sample analysis*
    LI Hai-lan, LIU Yu-ping, YAO Jian-neng, LIU Ying-ling, LI Ji
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 739-753. https://doi.org/10.16155/j.0254-1793.2024-1062
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    The components of biological samples are complex, and the concentration range of target analytes varies significantly. Therefore, sample pretreatment is particularly important for subsequent analysis. With the continuous development of analytical techniques, the requirements for sample pretreatment are also increasing. Pretreatment technologies are evolving towards microscale, time-saving, high-efficiency, online, and environmentally friendly directions to meet the requirements of complex matrices and trace analysis. Online pretreatment technologies integrate sample pretreatment steps and subsequent detection processes directly into an automated system, which can reduce steps and errors, improve analysis efficiency and sensitivity, and achieve automatic, rapid, and efficient analysis of target compounds. This paper reviews the online pretreatment technologies for biological samples in China and abroad in the past 10 years, offering valuable insights to guide future research and innovation in the realm of biological sample pretreatment.
    • Ingredient Analysis
  • Chemical components analysis of Bufei Jianpi formula based on UPLC-HRMS
    LIU Ze, ZHENG Li-shi, SHU Sheng-nan, SUN Shu-ding, LI Rong-rong, ZHAO Di, FENG Su-xiang
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 754-778. https://doi.org/10.16155/j.0254-1793.2024-1177
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To identify and analyze the chemical components of Bufei Jianpi formula by ultra-high performance liquid chromatography-coupled with high-resolution mass spectrometry (UPLC-HRMS). Methods: A Hypersil GOLD (2.1 mm×100 mm, 2.6 μm) column was used. Methanol (A)-0.1% formic acid water (B) was used as the mobile phase with gradient elution, the flow rate was 0.2 mL · min-1, and the column temperature was 30 ℃.The mass spectrometry data were collected using the Full MS/dd-MS2 scanning mode of positive and negative ions, and the characteristic fragment ion peak information was analyzed by compound discoverer. Combined with Chemspider, mzCloud and other databases and existing reports of relevant chemical composition information, the chemical components of Bufei Jianpi formula was analyzed by using the cracking prediction of Mass Frontier and its cracking rule. Results: A total of 221 compounds were identified from Bufei Jianpi formula, including 65 flavonoids, 40 phenylpropanoids, 21 terpenoids, 16 alkaloids and 79 other compounds. Conclusion: UPLC-Orbitrap Fusion Lumos Tribrid-MS can quickly identify the chemical components of Bufei Jianpi formula and qualitatively analyze the material basis of Bufei Jianpi formula, which can be used for the quality control of BufeiJianpi formula.
  • Simultaneous determination of fourteen active components in Qiyu Sanlong decoction by UPLC-QQQ MS/MS*
    WEI Zi-qi, YANG Rui, LI Lan-ying, JIANG Yu-ge, YANG Mo, ZHOU An, LI Ze-geng, WU Huan
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 779-795. https://doi.org/10.16155/j.0254-1793.2024-1216
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To establish an ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQ MS/MS) method for the simultaneous determination of 14 active components in Qiyu Sanlong decoction, including L-argnine, monotropein, deacetyl asperulosidic acid, rutin, peimisine, calycosin-7-O-β-D-glucoside, caffeic acid, solasonine, solamargine, p-coumaric acid, ferulic acid, calycosin, astragaloside Ⅳ and astragaloside Ⅰ. Methods: The chromatographic separation experiment was performed on an ACQUITY UPLC BEH C18 column(2.1 mm×100 mm, 1.7 μm), with gradient elution of 0.1% formic acid aqueous solution (A)-acetonitrile (B) as mobile phase at the flow rate of 0.2 mL · min-1, injection volume of 5 μL, and column temperature of 35 ℃. The ion source was an electrospray ionization source (ESI), the scanning mode was simultaneous scanning of positive and negative ions, and the monitoring mode was multiple reaction monitoring. Results: The 14 active components revealed good linearity within their respective ranges (r>0.995 0), RSDs of precision and repeatability were below 2%, RSDs of stability were below 3%, and the average recoveries ranged from 88.4% to 108.5% with the RSDs ranging from 0.020% to 3.6%. The content ranges of the aforementioned 14 components in 10 batches of self-prepared Qiyu Sanlong decoction were as follows (in μg · g-1): 667.28-785.78, 165.72-197.27, 196.32-275.60, 17.60-26.52, 4.68-10.75, 279.12-388.05, 26.00-47.57, 385.52-442.77, 288.00-358.82, 629.88-839.02, 86.67-125.83, 51.58-65.83, 25.50-37.53, and 55.50-76.13. Conclusion: The UPLC-QQQ MS/MS method established in this study is rapid, accurate, sensitive and repeatable, which can provide a reference for the quality control of Qiyu Sanglong decoction.
  • Simultaneous determination of eleven constituents in Jinlian Quwen capsules by HPLC*
    LIU Yi-fei, TU Wan-qian, ZHANG Liu-ji, LI Kai-yan, ZHANG Di-wen, YANG Dan
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 796-801. https://doi.org/10.16155/j.0254-1793.2024-1361
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To establish an HPLC method for the simultaneous determination of chlorogenic acid, puerarin, 3’-methoxy puerarin, puerarin apioside, liquiritin, forsythoside A, 3,5-O-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid, forsythin, honokiol and magnolol in Jinlian Quwen capsules. Methods: The analysis was performed on a Waters AtlantisTM T3 (150 mm×4.6 mm, 3 μm) column, and the mobile phase was comprised of acetonitrile-0.1% phosphoric acid, with the flow rate of 1.0 mL · min-1 in a gradient elution manner. The column temperature was set at 35 ℃. The injection volume was 4 μL and the UV detection wavelengths were set at 225 nm (detecting forsythin), 250 nm (detecting puerarin, 3’-methoxy puerarin and puerarin apioside), 276 nm(detecting liquiritin), 290 nm (detecting honokiol and magnolol) and 325 nm (detecting chlorogenic acid, 3,5-O-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid and forsythoside A). Results: All the 11 constituents showed good linearity within their detection ranges (r≥0.999 5), whose average recoveries (n=6) were 100.1%-108.1%, with the RSDs of 2.8%-4.1%. The content ranges of 11 components in three batches of samples were 7.505-7.606 mg · g-1, 3.485-3.920 mg · g-1, 0.969-1.068 mg · g-1, 0.837-0.955 mg · g-1, 1.009-1.436 mg · g-1, 3.037-3.602 mg · g-1, 5.259-5.371 mg · g-1, 0.931-1.012 mg · g-1, 1.428-2.053 mg · g-1, 0.939-1.018 mg · g-1 and 2.744-2.827 mg · g-1, respectively. Conclusion: The method is simple, sensitive and reliable. It can be used as a reference for the establishment of quality standard of Jinlian Quwen capsules.
  • Rapid identification of the chemical components in the Sishen pills based on UHPLC-Q TOF MS/MS and feature-based molecular networking*
    YU Shu-ting, WU Wei-wei, YE Gui-fang, SHI Jing-chao, QIN Xue-mei, LI Zhen-yu
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 802-820. https://doi.org/10.16155/j.0254-1793.2024-0507
    Abstract ( ) Download PDF ( )   Knowledge map   Save
    Objective: To establish a rapid analytical method for chemical components in complex traditional Chinese medicine (TCM) based on an integrated strategy combining ultra high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UHPLC-Q TOF MS/MS) with feature-based molecular networking (FBMN), so as to systematically characterize the chemical components in Sishen pills. Methods: MS data for Sishen pills were acquired using UHPLC-Q TOF MS/MS, with separation performed on on a Waters HSS T3 column(2.1 mm×100 mm, 1.8 µm). The mobile phase was consisted of a gradient elution of 0.1% formic acid in water (A) and acetonitrile (B) at a flow rate of 0.3 mL · min-1. The electrospray ionization (ESI) source was used for both positive and negative ion modes, with a scan range of m/z 80 to 1 500. The data were uploaded to the Global Natural Product Social Molecular Networking (GNPS) to create a FBMN for Sishen pills. Results: A total of 131 compounds were identified in Sishen pills, by analyzing retention time, accurate molecular mass, MS2 fragmentation characteristics, comparison with reference standards and self-established database, as well as utilizing FBMN for predicting structural similarity of compounds. These compounds included 27 alkaloids, 63 flavonoids, 11 phenylpropanoids, 14 phenols, 8 terpenoids, and 8 other compounds. Conclusion: In this study, the chemical components of Sishen pills are quickly and comprehensively characterized, which layes a foundation for the effective materials and quality control research of Sishen pills. The study also provides insights for the rapid analysis of chemical constituents in other TCM formulas.
  • Application of TRSDMC method for the determination of 5 components in Moslae Herba*
    LIU Li-qin, XU Zai-ping, FU Wen-yan, YUAN Ming-ming, ZHAO Wen, YANG Xin-kai, WAN Lin-chun, WEI Feng
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 821-832. https://doi.org/10.16155/j.0254-1793.2024-1039
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    Objective: To establish a two reference substances for determination of multiple components (TRSDMC) method for the simultaneous determination of scutellarin, rosmarinic acid, negletein, carvacrol and thymol in Moslae Herba, which was more economical and effective for the quality control of Moslae Herba. Methods: The retention times of the five components in Moslae Herba were determined using HPLC on 13 different C18 columns. The average retention time of each component under each column was then used as the standard retention time for that component. Rosmarinic acid (peak 2) and carvacrol (peak 4) were chosen as linear calibration standards. The chromatographic peaks were localized by using liner calibration with two reference substances (LCTRS). Rosmarinic acid was used as the control substance to determine the content of each component using a relative correction factor. And the results were compared with those obtained from the external standard method. Chemometric analysis was used to excavate the differential quality markers of Moslae Herba. Results: LCTRS had accurate prediction results for the measured components and enjoyed a wide range of column applications. The correction factors of scutellarin, negletein, carvacrol and thymol to rosmarinic acid were 0.853 3, 0.475 2, 3.034 7 and 2.738 6, respectively, and their relative standard deviations were below 2.0%. There was no significant difference between contents obtained by the two methods. The contents of scutellarin, rosmarinic acid, negletein, carvacrol and thymol in 21 batches of Moslae Herba were 0.05-2.87 mg · g-1, 0.73-9.73 mg · g-1, 0.04-0.99 mg · g-1, 0.36-8.52 mg · g-1 and 0.61-10.2 7 mg · g-1, respectively. The 24 batches of samples could be clustered into three categories, and thymol, carvacrol and negletein ether could be used as differential quality markers. Conclusion: TSDMC method for the simultaneous determination of the contents of 5 components in Moslae Herba is stable and reliable, and provides a new idea for the overall quality control of Moslae Herba.
  • Comparative study on the components of Kehuang capsules before and after fermentation based on multi-component content determination and chemometrics*
    WANG Yu-xia, HOU Jia-hao, LI Ran, TU Tian-zhi, SONG Yong-xing, DUAN Xu-hong, MA Dong-lai, WANG Qian
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 833-842. https://doi.org/10.16155/j.0254-1793.2024-1143
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    Objective: To compare the chemical composition changes in Kehuang before and after fermentation using multi-component content determination combined with chemometric analysis. Methods: HPLC was employed using a ZORBAX Eclipse Plus C18 column (4.6 mm×250 mm, 5 μm). The mobile phase consisted of acetonitrile and 0.1% phosphoric acid aqueous solution, applied with gradient elution. The flow rate was set at 1.0 mL · min-1,the column temperature was maintained at 30 ℃, the detection wavelength was 203 nm, and injection volume was 10 μL. This method was applied to analyze the chemical compositions of Kehuang before and after fermentation and to establish their corresponding chemical fingerprint profiles. Quantitative determination was conducted for 11 chemical constituents, including chlorogenic acid, cimifugin, notoginsenoside R1, baicalin, berberine, quercetin, baicalein, wogonin, emodin, chrysophanol, and physcion. Furthermore, chemometric methods such as hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares discriminant analysis (OPLS-DA) were employed to distinguish and compare the samples before and after fermentation, with the aim of identifying key differential compounds. Results: Chemical fingerprint profiles were established for Kehuang before and after fermentation, with 22 common peaks identified. The fingerprints had good specificity and can be used for quality evaluation of Kehuang. The results of multi-component content determination and chemometrics analysis revealed significant differences in the content of notoginsenoside R1 (1.023-2.927 mg · g-1), scutellarein (0.125-0.568 mg · g-1), and berberine hydrochloride (2.151-3.068 mg · g-1) among the crude Kehuang powder, fermented Kehuang powder, and the content of Kehuang capsules. Notoginsenoside R1, scutellarein and berberine were identified as differential markers between pre- and post-fermentation of Kehuang, which could serve as quality indicators for distinguishing and identifying Kehuang before and after fermentation. Conclusion: The chemical composition of Kehuang changes significantly after fermentation, and the differential compounds have been clearly identified, which provides an analytical basis for quality control in the production of Kehuangcapsules.
  • Development of the national standard materials of cyclosporine A, tacrolimus, sirolimus, and everolimus in frozen human whole blood*
    YU Ting, SHEN min, HUANG Jie, ZHANG Tian-jiao
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 843-850. https://doi.org/10.16155/j.0254-1793.2024-0108
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    Objective: To establish the national standard materials of cyclosporine A, tacrolimus, sirolimus, and everolimus in frozen human whole blood. Methods: Anticoagulated whole blood samples were collected without obvious hemolysis, jaundice, or lipemia. The whole blood samples that had tested negative for four infectious diseases were pooled. They were frozen at - 20 ℃ for more than 48 h. After thawing, the samples were centrifuged at 4 000×g for 10 min, the precipitate was discarded, and pure raw materials of cyclosporine A, tacrolimus, sirolimus, and everolimus were added to prepare the target concentrations. The mixture was mixed thoroughly and then aliquoted into ampoules at two concentration levels. The homogeneity and stability of the standard materials were evaluated using one-way analysis of variance and linear regression methods. The assigned values were determined by reference methods, and uncertainty was calculated. Finally, the commutability of the standards was evaluated. Results: The F values of the homogeneity for cyclosporine A, tacrolimus, sirolimus, and everolimus at level I were 1.492 1,1.395 6, 1.432 8, and 1.060 2, respectively, and at level Ⅱ were 1.441 2, 1.476 1, 1.458 0, and 1.454 6, respectively. All of them were less than F0.05. Level Ⅰ standard materials were stable for 10 d at 20-25 ℃ and 2-8 ℃, and for 30 d at - 20 ℃; Level Ⅱstandard materials were stable for 10 d at 20-25 ℃ and for 30 d at 2-8 ℃ and - 20 ℃. The assigned values of standard (k=2) were as follows: cyclosporine A level Ⅰwas (105.6±8.9) ng · mL-1, level Ⅱ was (419.8±32.8) ng · mL-1; tacrolimus level Ⅰwas (5.4±0.4) ng · mL-1, level Ⅱ was (17.0±1.8) ng · mL-1; sirolimus level Ⅰ was (5.0±0.3) ng · mL-1, level Ⅱ was (15.7±1.1) ng · mL-1; everolimus level Ⅰ was (4.8±0.2) ng · mL-1, level Ⅱ was (10.2±0.6) ng · mL-1. The two levels of standard concentration are within the 95% confidence interval of the regression line for fresh whole blood samples, indicating good commutability. Conclusion: The batch of the national standard material of cyclosporine A, tacrolimus, sirolimus, and everolimus in frozen human whole blood is homogeneous, stable, and commutable. The assigned values are accurate and reliable, and can be used as national standard for calibration of these four immunosuppressive agents, thereby promoting the standardization and consistency of test results.
  • Establishment of the first batch of national reference standards for bivalirudin*
    REN Li-ping, HE Lan-ying, LIAO Hai-ming, WANG Jin, YANG Hong-miao, FAN Hui-hong
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 851-858. https://doi.org/10.16155/j.0254-1793.2024-0274
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    Objective: To develop the first national reference standards for the quantitative determination of bivalirudin, in order to effectively control the product quality of bivalirudin injections, and to explore alternative methods for the quantitative characterization of synthetic peptide reference materials. Methods: Infrared (IR) spectroscopy, UV spectroscopy, HPLC, MS were used to confirm the structure of bivalirudin. Related substance were analyzed by HPLC. The mass balance method was used to determine the content of bivalirudin, which was further verified by a peptide content assay corrected for related peptide impurities. In addition, the stability and uniformity of the candidate reference material were evaluated. Results: The content of the first batch of bivalirudin national reference standard was 88.8%, calculated on C98H138N24O33, and the stability and uniformity tests met the required specifications. Conclusion: Based on the structural characteristics of the synthetic peptides, multiple qualitative and quantitative methods were used to ensure the accuracy of the content assignment for the national reference standard of bivalirudin.
    • Bioassay
  • Preparation of genistein monoclonal antibody and establishment of indirect competitive ELISA*
    LI Hua-yuan, GUO Yu, XIE Wei, XIANG Qian, ZHANG Wen, CAO Ya-jing, WANG Jing, LU Yan-yun, DUAN Si-qi, SUN Ying
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 859-866. https://doi.org/10.16155/j.0254-1793.2024-0492
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    Objective: To prepare monoclonal antibodies (MAbs) that can specifically recognize genistein (Gen), and to establish a specific and rapid quantitative method for Gen using indirect competitive enzyme-linked immunosorbent assay (ELISA). Methods: Gen was coupled with carrier protein by the Mannich method to synthesize artificial antigens. Femal Balb/c mice aged 6-8 weeks old were immunized by Gen-BSA. After the booster immunization, splenocytes of the mice were collected and fused with SP2/0 myeloma cells under the action of 50% polyethylene glycol (PEG). Subclones were screened by the limiting dilution method to obtain specific MAbs and an indirect competitive ELISA method was established. Results: Two hybridoma cell lines (C1 and C3) were isolated successfully with the titers of 1 ∶ 32 000, 1 ∶ 40 000, respectively. Under the optimized conditions, the indirect competitive ELISA based on C3 for Gen showed a half maximum inhibition concentration (IC50) of 16.15 ng · mL-1 and detection ranges of 3.78-55.85 ng · mL-1 with cross-reactivity for biochanin A and irisolidone of 4.96% and 2.40%, respectively, negligible cross-reactivity with other Gen analogs including apigenin and 4-oxo-4H-1-benzopyran-2-carboxylic acid. The recovery test showed that the recovery rate was between 85% and 110%, precision tests showed RSD of inter-assay and inter-assay was less than 10%. Conclusion: In this study, Gen-specific MAbs are prepared successfully. An sensitive and accurate indirect competitive ELISA based on MAb for Gen is developed. The developed method can meet the requirements for immunoassay.
  • Application of genetic antimicrobial susceptibility testing in the development of selective medium for the enumeration of multi-strain microecological preparation
    XING Sheng, FENG Dan-yang, SHEN Zhen, HU Wen-hong, LI Ying, DING Bo
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 867-879. https://doi.org/10.16155/j.0254-1793.2024-1097
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    Objective: To establish a selective culture medium screening method for counting viable bacteria from multi-strain microecological preparation based on gene and metabolic pathway analysis, in order to solve the problem of mutual interference in the measurement of counting viable bacteria. Methods: By analyzing the genomic scale metabolic network, the antibiotic sensitivity and resistance of Bacillus cereus, Enterococcus faecalis, Lactobacillus acidophilus, and Bifidobacterium infantis were quickly predicted. Based on the prediction results, suitable types and concentrations of antibiotics with resistance differences among the four microorganisms were screened and added to the culture medium, effectively inhibiting the growth of interfering microorganisms and ensuring accurate and effective counting results. Simultaneously, conventional drug sensitivity experiments results were used to ensure and compare with this method. Results: In the process of viable counting for multi-strain microecological preparation, this method effectively eliminated the interference of Enterococcus faecalis on the counting of Lactobacillus acidophilus live bacteria and the interference of Lactobacillus acidophilus and Enterococcus faecalis on the counting of Bifidobacterium infant, and the counting results were accurate and reliable of each microorganism. Conclusion: The method has strong foresight and specificity. Genomic analysis and metabolic pathway analysis can effectively predict microbial antibiotic resistance, and experimental design based on the predicted results will greatly accelerate experimental efficiency, making the results more predictive and accurate, and has broad application prospects in selective culture medium screening for counting viable bacteria from multi-strain microecological preparation.
    • Safety Monitoring
  • Content determination of impurity elements in gadolinium-based contrast agent by inductively coupled plasma tandem mass spectrometry*
    NI Bi-yu, CHEN Lin, ZHENG Chao, HUANG Jian-hua, XIE Wen
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 880-888. https://doi.org/10.16155/j.0254-1793.2024-1229
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    Objective: To meet the needs of gadolinium-based contrast agent (GBCA) analysis and testing, and to ensure drug quality and safety, a new strategy for inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) determination of 12 impurity elements (Cr, Fe, Co, Ni, Cu, V, Zn, As, Cd, Ba, Sb, and Pb) in GBCA was proposed. Methods: GBCA was diluted with 2% HNO3 and directly analyzed by ICP-MS/MS. Spectral interferences from V, Cr, Fe, Co, Ni, and Cu were eliminated using cool plasma/NH3/He reaction mode. In addition, spectral interferences from Zn, As, Cd, Ba, and Sb were eliminated using hot plasma/O2/H2 reaction mode. To evaluate the accuracy and reliability of the method, the standard reference material (NIST SRM 1643f) was analyzed by comparing the method with high-resolution ICP-MS (HR-ICP-MS), and the spiked recovery experiment was conducted. Results: Under optimized conditions, the limits of detection (LOD) of the analytes were 0.014-0.86 ng · L-1, the spiked recoveries were 96.7%-105.8%, and the RSDs were 1.6%-4.0%. The HR-ICP-MS determination values were consistent with reference values of NIST SRM 1643f. Statistical analysis showed that there was no significant difference between the measured values of the two methods at a 95% confidence level. Conclusion: The analysis method is accurate, reliable, stable and high precision. The combination of ICP-MS/MS and various reaction modes under different plasma conditions has shown promotion value for multi-element analysis in GBCA and can be extended to other fields.
  • UPLC-QQQ MS/MS with solid phase extraction for simultaneous determination of 68 veterinary drug residues in Galli Gigerii Endothelium Corneum*
    LIU Meng, ZHANG Liang, CHEN Fang-fang, LI Zhi-mei, ZHANG Chong-sheng
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 889-900. https://doi.org/10.16155/j.0254-1793.2024-1214
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    Objective: To establish a method for the determination of veterinary drug residues in Galli Gigerii Endothelium Corneum by ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-QQQ MS/MS) with solid-phase extraction. Methods: The samples were evenly dispersed, extracted with acetonitrile and acetonitrile containing 0.5% formic acid, and cleaned up with Oasis PRiME HLB solid phase extraction columns. The extracts were separated on Agilent ZORBAX Eclipse Plus C18 (3.0 mm×150 mm, 1.8 μm) using 5 mmol · L-1 ammonium acetate and acetonitrile (containing 0.1% formic acid) as mobile phase by gradient elution. The detection of veterinary drug residues was detected by tandem mass spectrometry with positive electrospray ion source under multiple reaction monitoring (MRM) mode. The matrix-matched external standard method was used for the quantitation. Results: The method exhibited good linearities within a certain concentration range r≥0.995 8. The limits of detection (LODs) were in the range of 0.1-3 μg · kg-1. The limits of quantitation (LOQs) were in the range of 0.2-10 μg · kg-1. The good recovery values (61.9%-121.5%) were achieved for all the 68 veterinary drugs with RSDs ranging from 0.50% to 8.4% for spiking 3 different levels. Out of 50 batches of samples, 5 batches of Galli Gigerii Endothelium Corneum were found to contain veterinary drug residues, including amantadine, doxycycline, enrofloxacin, and florfenicol. Conclusion: This method proves suitable for the rapid determination of multiple veterinary drug residues in Galli Gigerii Endothelium Corneum, with a simple, quick, accurate and procedure.
  • Determination of 8 elemental impurities in lanthanum carbonate with ICP-MS standard addition method and matrix matching method
    DING Fang-fang, SUO Zhe-dan, ZHENG Jin-qi, AI Jie, GU Xiao
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 901-906. https://doi.org/10.16155/j.0254-1793.2024-1073
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    Objective: To develop an inductively coupled plasma mass spectrometry(ICP-MS) method for the determination of Cd, Pb, As, Hg, Co, V, Ni and Se in the crude drug of lanthanum carbonate. Methods: Samples were diluted with 3% nitric acid and directly injected. The matrix effect was eliminated by standard addition method and matrix matching method. Lanthanum oxide was added into the standard solution as the matrix. Compare the linearity, repeatability, accuracy, quantification limit, detection limit and sample determination results of the two methods by methodological validation and sample determination. Results: The linear ranges of ICP-MS standard addition method and matrix matching method were 0-30 ng · mL-1, the correlation coefficients for all elemental impurities were good(r>0.998). Limits of detection were between 0.003 9-0.22 ng · mL-1 and 0.009 1-0.72 ng · mL-1. The RSD of repeatability(n=6) were between 1.5%-4.9% and 5.1%-6.9%. The recoveries were between 87.0%-98.3% and 83.4%-114.4%. The contents of 8 elemental impurities in the crude drug of lanthanum carbonate were basically same. Conclusion: The established two methods can effectively eliminate the matrix effect. They were both simple, rapid, sensitive, accurate and applicable for the elemental impurity control of lanthanum carbonate.
    • Standard Deliberation
  • Analysis of the impact of storage temperature on the critical quality attributes of terlipressin for injection*
    WANG Pei, LU Xin, MA Bing, DUAN Xi-yu, QIN Ting-ting, HAN Xiao-jie, BAI Hai-jiao
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 907-914. https://doi.org/10.16155/j.0254-1793.2024-1064
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    Objective: To clarify the differences between the “Room temperature” definitions in the European Pharmacopoeia and the Chinese Pharmacopoeia, to emphasize that storage temperature was closely related to the design of long-term stability studies and product labeling, and to investigate the effects of storage temperature variations on the critical quality attributes (CQAs) of terlipressin for injection, so as to raise awareness among generic drug manufacturers regarding this critical issue. Methods: Given the discrepancies in storage temperature recommendations across different manufacturers’ product inserts, the original drug’s long-term stability studies and storage conditions were traced. Validated methods for related substances and polymer content were employed to assess the impact of temperature differences on the product’s CQAs. Results: Samples stored at 30 ℃exhibited a significantly higher increase in related substances compared to those stored at 15 ℃. In one manufacturer’s product, polymer levels exceeded specification limits within just five months of storage at 30 ℃. The divergence among manufacturers stems from some companies misinterpreting the original drug’s labeling by directly translating without considering the differences between Chinese and European Pharmacopoeias. Conclusion: Storage temperature has a significant impact on the levels of related substances and polymer content in terlipressin for injection. To ensure product quality, the storage temperature in the labeling should be restricted to “not exceeding 25 ℃.”
  • Analysis of the influence of adsorbed moisture on DSC method for detecting drug purity
    LIU Yi, WU Rui, GUO Xian-hui, ZHU Jiong, CHEN Hua
    Chinese Journal of Pharmaceutical Analysis. 2025, 45(5): 915-920. https://doi.org/10.16155/j.0254-1793.2024-1249
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    Objective: To investigate the effect of adsorbed moisture on drug purity determination by differential scanning calorimetry (DSC). Methods: The DSC analysis for drug purity was performed with a heating rate of 0.5 ℃ · min-1 under a nitrogen atmosphere (drying gas flow rate: 50 mL · min-1). The optimized method reduced by 10 ℃ than the conventional method and included an additional heating segment at 1 ℃ · min-1 for 10 min, while other parameters remained unchanged. Results: Without pre-drying, the conventional DSC method accurately determined the purity of imidazole, phenylephrine hydrochloride, and neostigmine methylsulfate samples with adsorbed moisture below 7%. After optimization, the method further eliminated moisture interference, allowing accurate analysis of samples with adsorbed moisture below 8%. Conclusion: Adsorbed moisture may affect DSC-based purity analysis. For general samples with a melting point above 80 ℃ and adsorbed moisture below 7%, pre-drying is unnecessary. The optimized method further reduces the impact of adsorbed moisture.
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