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.

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.

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.

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 ℃.”

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.

Oligosaccharides are a class of bioactive components abundantly found in Chinese herbal medicine. They have clinical effects such as antidepressant and anti-Alzheimer’s disease activities, as well as pharmacological activities such as hypoglycemic, laxative, and immune-enhancing effects. The bioactivity of oligosaccharides is closely related to their structure. However, due to the diversity of glycosidic bond configurations, monosaccharide compositions and linkage patterns, it is difficult to accurately determine their structures by conventional analytical methods. Establishing rapid and reliable analytical methods remains a key challenge in carbohydrate research.Although studies on oligosaccharides are increasing, there is a lack of comprehensive reviews on the structure and analytical methods of oligosaccharides in Chinese herbal medicine. This paper systematically reviewed the research progress over the past decade on extraction, separation, structure identification and analytical methods of oligosaccharides in Chinese herbal medicine by consulting domestic and foreign literatures. This review aims to contribute to the development of evaluation method of traditional Chinese medicine based on oligosaccharide components, and provide reference for their application in the quality control of traditional Chinese medicine.

Objective: To analyze six components in Bletillae Rhizoma using high-performance liquid chromatography. Through the linear calibration using two reference substances method, the retention time of the components was predicted, and the feasibility and accuracy of this technique in the qualitative identification of chromatographic peaks were explored. This method was also compared with the relative retention time (RRT) method. Methods: High-performance liquid chromatography was employed using an Ultimate XB-C₁₈ column (250 mm×4.6 mm, 5 μm). The mobile phase consisted of water (A) and acetonitrile (B), with a gradient elution as follows: 0-11 min,12% B; 11-58 min, 12% B to 68% B; 58-65 min, 68% B to 12% B. The flow rate was 0.9 mL · min^-1, the injection volume was 5 μL, the column temperature was maintained at 30 °C, and the detection wavelength was set at 280 nm. By measuring the actual retention time of the six components on 16 different C₁₈ chromatographic columns, the standard retention time was calculated. Gastrodin (Peak 1) and gymnadenin Ⅲ (Peak 4) were used as the double-standard compounds.The linear calibration using two reference substances method was used to predict the retention time of other components,and the prediction was verified on another three unknown C₁₈ chromatographic columns. With the relative retention time(RRT) method, using bletilloside (Peak 5) as the reference compound, the retention times of the other five components were predicted. Results: A qualitative analysis method for the six components in Bletillae Rhizoma was established,which could accurately predict the retention times of each component in Bletillae Rhizoma. The standard retention times of the six components as as follows: gastrodin 4.279 min, gymnadenin Ⅲ 32.145 min, pleione bulbocodioides factor Ⅰ27.220 min, 2-O-glucosylbletilloside 28.603 min, bletilloside 33.509 min, and batatasin Ⅲ 45.504 min. Conclusion: The linear calibration using two reference substances method can improve the prediction ability of the retention time of each component in Bletillae Rhizoma, thereby enhancing the accuracy and reliability of the analysis results.

Objective: To establish an ultra-high performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）method for the simultaneous determination of 22 components of Bimin capsules, including benzoylaconine, benzoylmesaconine, benzoylhypacoitine, hypaconitine, mesaconitine, fuziline, aconitine, aconine,mesaconine, isoliquiritigenin, echinatin, protocatechuic acid, liquiritigenin, isoliquiritoside, glycycoumarin,naringenin, schaftoside, licochalcone B, glycyrrhizic acid ammonium salt, liquiritin, liquiritin apioside and isoliquiritin apioside. Methods: The Acclaim^TM RSLC 120C₁₈ column (2.1 mm×100 mm, 2.2 μm) was used with 0.05% formic acid water (A) and acetonitrile (B) as the mobile phase at a flow rate of 0.4 mL · min^-1. Electrospray ionization (ESI) source and multiple reaction monitoring (MRM) mode in both positive and negative were used for ion detections. Resulets:The 22 components displayed a good linear relationship (R²>0.990) in their respective ranges, and the precision, repeatability, stability, and sample recovery rate all met the requirements. It was found that all 22 components were detected in the nasal sensitivity capsules, with significant differences in the content of some components. Conclusion: This method is fast, simple, sensitive and reliable, and can provide scientific basis for the quality control of the Bimin capsules.

Objective: To establish the UHPLC fingerprint and quantitative analysis of CBDA, CBD, THC, and THCA for hemp, and provides a basis for the quantity control of hemp. Methods: UHPLC was launched on a Phenomenex C₁₈ (150 mm×4.6 mm, 2.6 μm) with mobile phase of acetonitrile-0.2% phosphoric acid aqueous solution at a flow rate of 1.0 mL · min^-1, column temperature of 35 ℃, detection wavelength of 220 nm, and an injection volume of 2 μL by gradient elution. 15 batches of hemp samples from Daxing ’anling region and Qiqihar were analyzed to establish the fingerprint. Cluster analysis, principal component analysis and orthogonal partial least squares discriminant analysis were adopted to assess of UHPLC fingerprint of hemp. Results: the UHPLC fingerprint of hemp was established, and 26 common peaks were selected the 26 common peaks were compared with the reference substance. The structures of four chromatographic peaks were identified and simultaneously analyzed for content determination. four chromatographic peaks were identified as CBDA, CBD, THC and THCA.The similarity of fingerprint of them was greater than 0.950. The samples from Daxing’anling were clustered into class Ⅰ, with the best quality. The results show that hemp samples from different regions were quite different. The variable importance projection (VIP) showed that the four compounds to be tested were the main components leading to the difference of hemp. Conclusion: The established method is stable and reliable and can be used for qualitative and quantitative analysis of hemp. The findings of this study are expected to provide a scientific basis for quality control of hemp.

Objective: To explore the growth trend of volatile components in hawthorn fruit at different growth stages. Methods: The volatile components in hawthorn fruits at different growth stages were quantitatively and qualitatively analyzed by gas chromatography-mass spectrometry (GC-MS), and their dynamic changes were investigated and statistically analyzed. The chromatographic column used was HP-5 (30 m×0.32 mm, 0.25 μm),while the column temperature was programmed (initial temperature 60 ℃, increased to 250 ℃ at a rate of 10 ℃ · min^-1,maintained for 33 min), and the inlet temperature was 280 ℃. The ion source was an electron bombardment source(EI), with an ion source temperature of 230 ℃. Results: A total of 57 representative volatile components were detected,of which 16 components disappeared in the later stage of growth, and 12 components were not present in the early stage of growth. The content of 11-decyl-tetracosane was the highest and gradually increased, and the content of hexadecyl acrylate gradually decreased. Conclusion: The investigation of the dynamic changes of volatile components in hawthorn fruit during the growth period provides a reference for further rational development and utilization of hawthorn fruit.