Lonicera japonica is a kind of medicinal plant with a long history of medicinal and edible homology, which is widely distributed and has significant pharmacological activity. L. japonica contains abundant phenolic acids, flavonoids, iridoid, triterpenoid saponins, volatile oils and other active ingredients, which have antioxidant, antibacterial, antiviral and other pharmacological activities. Through consulting multiple literature databases such as Jihn.com, Wanfang and X-mol, the main literature in the past five years was mainly cited. The main active components in L. japonica, rattan and leaves and the pharmacological activities of L. japonica extract were summarized, which provided reference for the comprehensive exploitation and deep processing of L. japonica.

Therapeutic oligonucleotides (OGNs) drugs are artificially synthesized single or double stranded short nucleic acids, typically 15 to 30 base pairs in length. OGNs have been rapidly developed as new therapeutic drugs with increasing attention in the discovery and development of drugs concerning various disease fields. Compared with Europe and America, there are currently no other OGNs drugs listed in China, except for Spinraza, which has been approved for marketing as an orphan drug. The development of OGNs in China started relatively late and is still in its early stages of development. However, the OGNs drug market in China is anticipated to grow quickly due to the country's large population, high patient demand, ongoing support for the development of oligonucleotide drugs in the future, and the steady maturation of related technologies by domestic businesses. Because of their special physicochemical characteristics, OGNs drugs are challenging to design biological analysis techniques. Currently, there are few reports on quantitative analysis methods for oligonucleotide drugs in China. Therefore, the development of sensitive and reliable bioanalysis methods for oligonucleotides is the key to investigate oligonucleotides' pharmacokinetic and pharmacodynamic properties. Liquid chromatography-mass spectrometry (LC-MS) can quantify OGNs and their metabolites concurrently, compared with traditional ELISA approaches. Numerous benefits come with using LC-MS, in particular, the extensive use of high-resolution mass spectrometry allows for the identification of metabolites, which provides details on base composition and sequence structure, in addition to quantitative information about target oligonucleotides. It has now emerged as the go-to technique for OGN quantitative analysis. The application of LC-MS in the identification of therapeutic oligonucleotide medicines is the primary focus of this paper, which also discusses its benefits and drawbacks. Lastly, it looks at the LC-MS development trend for oligonucleotide detection, which includes a lower detection level and potential general methods.

Gas chromatography-Orbitrap mass spectrometry (GC-Orbitrap/MS), a developing gas chromatography-high resolution mass spectrometry approach, allows for high throughput qualitative and quantitative analysis of volatile and semi-volatile components. It has the advantages of high sensitivity, selectivity, and a wide linear dynamic range, which makes it well suitable for the analysis of a wide range of trace substances in complex matrices. In recent years, this technology has been applied in environmental science, industry, food analysis, pharmaceutical analysis, forensic science, clinical medicine and other fields. This paper presents the first review of GC-Orbitrap/MS, which not only describes the basic principles and technical characteristics, but also introduces the progress of the technique in food and pharmaceutical research. Applications in food analysis include the inspection of pesticide residues, detection of persistent organic compounds and analysis of flavor substances. In pharmaceutics, the analysis of chemical impurities and quality evaluation of traditional Chinese medicine are introduced. It is noteworthy that this technique is particularly advantageous for the identification of unknown compounds and the determination of ultra-trace components. Lastly but importantly, this review summarizes the challenges encountered in the current development of this technique, including the establishment of high-resolution standard databases, the selection and optimization of sample pre-treatment method and the application of GC-Orbitrap/MS in the field of traditional traditional Chinese medicine. A few solutions are also proposed, such as the application of variable electron voltage technique, the combination of two-dimensional gas chromatography and electrostatic field Orbitrap mass spectrometry and the integrated analysis comprehensively using multiple scan modes. These strategies are aimed to provide more advanced and accurate solutions to food, pharmaceutical, and other relevant analysis.

Patch refers to a thin sheet flexible preparation made of raw drug and suitable material for sticking on the skin, which can produce systemic or local effects. In vitro release test (IVRT) and in vitro permeation test (IVPT) are important contents of preclinical pharmaceutical research for formulation process optimization, quality control and safety and effectiveness evaluation of patch. The experimental equipment and methods used are different, the obtained experimental samples and data are different from each other, and the accuracy and precision of the experimental data are also different. Therefore, the selection of experimental equipment and the establishment of experimental methods in the in vitro experiment of IVRT & IVPT is a problem worthy of attention. In this paper, the research status of patch was summarized, the requirements of pharmacopoeia of different countries for IVRT experiments were briefly introduced, and the differences of different methods were reviewed. For IVPT experiments that have not yet been prescribed by relevant standards, the common types of experimental equipment and experimental conditions were introduced in detail, the applicability of different equipment and the influence of main experimental conditions (temperature, stirring speed, composition of acceptor solution, selected skin, etc.) on the experimental results were summarized, and the research progress of in vivo and in vitro correlation was introduced. At the same time, the validity of the experimental data was discussed, hoping to provide a useful reference for the development and research of the in vitro experimental methodology of the patch.

The national drug sampling and inspection project is an important way of drug quality supervision in China which providing strong support for drug supervision and standard improvement. This article summarizes the national drug sampling and inspection project of Arnebiae Radix completed by Institute for Control of Chinese Traditional Medicine and Ethnic Medicine, National Institutes for Food and Drug Control in 2015 and 2022. The results illustrated that the qualification rate of Arnebiae Radix has increased from 43.9% in 2015 to 87.5%, and the qualification rate of Arnebiae Radix has significantly increased. The two nationwide inspections of Arnebiae Radix reflected the scarcity of Arnebiae Radix resources in Xinjiang and Inner Mongolia, resulting in a high market share of unqualified samples. The thin layer identification spots of the unqualified Arnebiae Radix sampled in 2015 were not consistent with the qualified samples. The thin layer identification of the unqualified samples sampled in 2022 was consistent with those of the qualified samples, but the depth of the spots were not consistent with those of the qualified samples, indicating that the current unqualified samples were adulterated samples, which posing greater challenges to the quality supervision of Arnebiae Radix. Through the exploratory research of twice National Drug Sampling and Inspection Project, it is preliminarily believed that it is of great significance to improve the standard test items of Arnebiae Radix, scientifically establish the limit value and strengthen the construction of the quality control system for the supervision.

Objective: To establish a three classification model for cultivated, semi-wild, and wild Astragali Radix characterized by flavonoids, and explore and evaluate the application of techniques of automated machine learning and data augmentation in the field of drug analysis. Methods: Firstly, correlation analysis and principal component analysis were conducted on the flavonoid content data of Astragali Radix, and models of decision tree and logistic regression were established to analyze the importance of flavonoid components based on the models. Then, using the AutoGluon framework with 5 as num_bag_folds, 2 sets of 30 models respectively through 64 batches of real data and 600 batches of virtual data generated based on real data with the TVAE table data generation algorithm for training were obtained, and these models were evaluated by accuracy. Results: The analysis of machine learning models, indicated that formononetin, campanulin and onospin played the important roles in the quality control of Astragali Radix, especially for the source grade control. The accuracy of model prediction showed that the models based on Neural Net and tree-model always had the best classification effect for Astragali Radix. The virtual data generated by data augmentation technique is basically consistent with the actual data in terms of the accuracy trend of the model training process. Conclusion: Related techniques of machine learning have good application value in the classification of Astragali Radix characterized by flavonoids.

CircRNAs are a large class of endogenous single-stranded RNAs that are different from other linear RNAs, which are produced by back-splicing and fusion of either exons, introns, or both exon-intron into covalently closed loops. They are widely expressed in highly differentiated eukaryotes, and are closely related to various development and metabolic disease processes of organisms. They are characterized by stable structure, resistant to RNA degradation, conservation, and tissue-specific expression, making them ideal biomarkers for diagnosis and prognosis. Traditional methods such as Northern blotting, qRT-PCR and microarray analysis provide useful information, however, they are subject to their own shortcomings. Traditional methods are restricted in large-scale promotion in clinical trials. In recent years, in order to solve these problems, some new detection methods have emerged. In this article, we reviewed the relevant progress of all current circRNA detection methods, expounded their advantages and limitations, and discussed the challenges and future development directions.

Thyroid-stimulating hormone (TSH) is a glycoprotein hormone produced by the anterior pituitary. It can regulate the synthesis and secretion of thyroid hormone in thyroid follicular cells, which has important physiological significance. As a drug, it has important application value. Biological activity detection is an effective and necessary to evaluate its quality. This article discusses the signal transduction mechanism of thyroid stimulating hormone, the clinical diagnosis and treatment of thyroid stimulating hormone, and the determination method of biological activity.

Objective: To determine seven impurities in oxytocin for injection and investigate the limit values. Methods: HPLC and principal component self-control with correction factor were adopted. The determination was performed on a Waters Xbridge C₁₈ column(150 mm×4.6 mm, 5 μm). The mobile phase consisted of 0.1 mol·L^-1 dihydrogen phosphate solution (adjusted to pH 5.4)-acetonitrile (90∶10, phase A), and acetonitrile (phase B) with gradient elution at a flow rate of 1.5 mL·min^-1. The column temperature was maintained at 32 ℃, and the detection wavelength was set at 220 nm. The injection volume was 100 μL. The linear equations of oxytocin, impurities Ac-Oxy, Oxy[Glu⁴], Oxy[+Gly¹⁰], Oxy[-NH₂], Oxy[trisulfide], Oxy[cis-dimer] and Oxy[trans-dimer] were drawn. The correction factors of each impurity related to oxytocin were calculated by slope. The contents of impurities in 3 batches of oxytocin for injection were determined and compared with the results of impurity reference method. Results: The limits of quantification for seven impurities were 2.75-5.66 ng, while the detection limits were 1.38-2.83 ng. The linear ranges of seven impurities were 0.03-3.40 μg·mL^-1 with good linearity(r>0.999). The correction factors of Ac-Oxy, Oxy[Glu⁴] and Oxy[-NH₂] were 1.1, while the correction factors of Oxy[+Gly¹⁰] and Oxy[trisulfide] were 1.2 and 0.9, respectively. The correction factors of Oxy[cis-dimer] and Oxy[trans-dimer] were both 1.3. The seven impurities were determined in 3 batches of samples by principal component self-control with correction factor. The contents of impurity Ac-Oxy were 0.96%,0.93% and 1.01%, respectively. The contents of impurity Oxy[Glu⁴] were 0.07%, 0.06% and 0.08%, respectively. The contents of impurity Oxy[+Gly¹⁰] were 0.07%, 0.04% and 0.04%, respectively. The contents of impurity Oxy[-NH₂] were 0.09%, 0.05% and 0.07%, respectively. The contents of impurity Oxy[trans-dimer] were 0.27%, 0.18% and 0.22%, respectively. The maximum single impurity contents were 0.18%-0.19%, while the total impurity contents were 1.88%-2.06%. Compared the results measured by principal component self-control with correct factor method and the impurity reference method, there was no significant difference between two methods (p>0.05). Conclusion: The method is proved to be simple, repeatable and accurate for the content determination of related substances in oxytocin for injection.

Objective: To establish a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous determination of atorvastatin, two activity-related hydroxy statin metabolites and three toxicity-related statin lactones in human plasma, and its application to the study of pharmacokinetics in healthy subjects and the analysis of concentrations in patients. Methods: After acidification, plasma samples were treated by protein precipitation. The LC separation was performed on a Zorbarx SB-C₁₈(50 mm×2.1 mm, 5 μm) column. Methanol-acetonitrile (1∶1) water-methanol-acetonitrile (9∶0.5∶0.5) containing 0.05% formic acid were used as the mobile phases for gradient elution, and the flow rate was 0.35 mL·min^-1. The electric spray ionization source, positive ion mode and multi-reaction monitoring scanning were adopted for MS detection. The m/z of each targeted analyte was 559.3→440.2 for atorvastatin, 575.1→440.3 for 2-hydroxy atorvastatin acid (2-HAT) and 4-hydroxy atorvastatin acid (4-HAT), 540.9→448.2 for atorvastatin lactone (ATL), 557.2→448.2 for 2-hydroxy atorvastatin lactone (2-HATL) and 4-hydroxy atorvastatin lactone (4-HATL), and 422.2→290.0 for the internal standard of pitavastatin. After a full method validation, the developed LC-MS/MS method was used to determine the plasma samples of healthy subjects and patients after taking atorvastatin calcium tablets, and the pharmacokinetic characteristics of atorvastatin and five metabolites were analyzed. Results: The calibration curves of atorvastatin and its metabolites presented a good linear relationship in the range of 0.1-25 nmol·L^-1. The RSD of intra-and inter-day precision and the RE of accuracy were all less than 15%, and the stability was well tolerated under different conditions. In healthy subjects after oral administration of 20 mg atorvastatin calcium tablets, the respective mean values of C_max for atorvastatin, 2-HAT, 4-HAT, ATL, 2-HATL and 4-HATL were 11.48, 4.71, 0.28, 1.71, 2.52 and 2.31 nmol·L^-1, AUC_0-∞ were 87.31, 58.79, 8.60, 28.75, 45.76, 31.49 nmol·h·L^-1, t_1/2 were 7.96, 7.93, 19.58, 8.76, 8.98 and 21.37 h. After 12 h of administration, the average blood concentrations of atorvastatin, 2-HAT, 4-HAT, ATL, 2-HATL and 4-HATL in the patient were (4.16±1.31) nmol·L^-1, (2.65±1.33) nmol·L^-1, (1.15±1.16) nmol·L^-1, (2.96±1.83) nmol·L^-1, (4.27±2.00) nmol·L^-1 and (3.70±1.74) nmol·L^-1. Conclusion: The method for the simultaneous quantitative determination of atorvastatin and five metabolites in human plasma established in this study is accurate, rapid, sensitive and stable, and can be used for clinical pharmacokinetics research and plasma drug concentration monitoring. The clinical studies revealed that toxicity related lactone metabolites have a high level of exposure in humans, which requires attention to the possible risk of side effects.

Objective: To improve the liquid chromatographic determination method of cefixime granules related substance. Methods: High performance liquid chromatography was used, YMC-Triart C₁₈ column (250 mm×4.6 mm, 5 μm) was selected, 0.05 mol·L^-1 ammonium formate solution (pH 4.7)-methanol was used as mobile phase, flow rate was 1 mL·min^-1, and gradient washing was carried out.The injection volume was 10 μL. The detection wavelength was 254 nm. Results: This chromatographic condition was applied to the detection of cefixime granules. The differences between this method, the pharmacopeial method and the method of USP PF 2018 were compared, and the systematic methodological verification of specificity, linearity, accuracy, precision and durability were completed. Using pharmacopeial methods, baseline separation of degradation impurities A1~A4 or impurities B1~B4 cannot be reached, and current methods cannot be used to determine polymer B and polymer D. The method proposed in this article can make the resolution between cefixime and each specific impurities meet the requirements (R ≥1.5), and can detect and quantify polymer B and polymer D at the same time, and the resolution was better than the current method. Conclusion: This method improves the separation between cefixime and impurities, more impurities is detected and can accurate quantify specific impurities. This method has high sensitivity and good repeatability, and is suitable for the quality control of cefixime.

Objective: To analyze the chemical constituents of Quyusanjie capsules by LC/MS, and establish a method for the determination of active ingredients in Quyusanjie capsules. Methods: Using UPLC-Q TOF MS/MS technology, the Hypersil Gold C₁₈ column(100 mm×2.1 mm,1.9 μm) was used, the mobile phase was acetonitrile(A) and 0.1% formic acid in water(B) with gradient elution, at a flow rate of 0.4 mL·min^-1, the the column temperature was 40.0 ℃, and the mass spectrometry data was collected by negative ions mode scanning. Through database matching, elemental composition and fragment structure analysis, the main chemical substances in Quyusanjie capsules were identified. HPLC was used to qualitatively analyze the chemical components of Quyusanjie capsules. The Ultimate^® AQ-C₁₈ column(250 mm×4.6 mm, 5 μm) was used, the mobile phase was acetonitrile(A)-0.1% phosphoric acid(B) with gradient elution at the flow rate of 1.0 mL·min^-1, the column temperature was 25 ℃, and the detection wavelength was 203 nm. The content of naringin, neohesperidin, notoginsenoside R₁, ginsenoside Rg₁, and ginsenoside Rb₁ in 11 different batches of Quyusanjie capsules were determined using external standard method. QAMS method was established using ginsenoside Rg₁ as the internal reference. Results: Twenty-nine compounds were identified from Quyusanjie capsule. The contents of naringin, neohesperidin, notoginsenoside R₁, ginsenoside Rg₁ and ginsenoside Rb₁ measured by external standard method were 0.484-1.097 mg·g^-1, 0.341-0.618 mg·g^-1, 1.685-2.399 mg·g^-1, 5.748-8.386 mg·g^-1, 3.868-5.898 mg·g ^-1, respectively. Measured with the QAMS method, the contents of naringin, neohesperidin, notoginsenoside R₁ and ginsenoside Rb₁ were 0.516-1.153 mg·g^-1, 0.372-0.667 mg·g^-1, 1.794-2.580 mg·g^-1, 4.373-6.690 mg·g^-1, respectively. The relative error between the calculated values of the QAMS method and the measured value of the external standard method was less than 8.9%. Conclusion: UPLC-Q TOF MS/MS method can quickly identify the chemical components of Quyusanjie capsules. The established external standard method is stable and reliable, and can be used for the quality control of Quyusanjie capsules. The method of QAMS has good feasibility and is suitable for the determination of the daily production of Quyusanjie capsules.

Objective: To develop a high performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method for the determination of vildagliptin in human anticoagulant plasma with ethylenediamine tetra acetic acid and apply it to the study of pharmacokinetics. Methods: ¹³C-¹⁵N-vildagliptin was used as internal standard (IS). After extraction from human plasma by protein precipitation with acetonitrile, all components were separated by a Hypurity C₁₈ column (150 mm×2.1 mm,5 μm), using a gradient elution procedure consisting of methanol and 5 mmol·L^-1 ammonium formate at a flow rate of 0.5 mL·min^-1,and the column temperature was 40 ℃. Injection volume was just 2 μL. Positive electrospray ionization was performed using multiple reaction monitoring (MRM) with transitions of m/z 304.3→154.2 for vildagliptin and m/z 310.3→160.3 for internal standard. Specificity,standard curve, lower limit of quantification,precision,recovery,matrix effect and stability were examined. Then this method was used to determine the plasma concentration of veragliptin in healthy subjects. Results: The calibration curve of vildagliptin in human plasma was linear over the concentration range of 1.11 to 534.0 ng·mL^-1. The lower limit of quantitation was 1.11 ng·mL^-1. The intra-and inter-day precisions at four quality control levels were within 0.9%-8.5%,and the accuracy was within 99.8%-109.3%. The data of short-term stability at room temperature displayed that the accuracy percentage of LQC samples was 92.0% for 0.5 h exposure, 87.6% for 1 h exposure, 71.2% for 2 h exposure. These of LQC samples chilled on ice was 102.0% for 0.5 h exposure, 94.5% for 1 h exposure, 86.6% for 2 h exposure. These results showed a phenomenon that there was a possible degradation of vildagliptin in plasma. The results of extraction recovery and matrix effect and other stability met the requirements of biological sample analysis. The pharmacokinetic study results of 8 healthy subjects showed that t_1/2 was (1.49±0.37) h, t_max was (2.06±1.11) h, C_max was (290.94±100.36) ng·mL^-1, AUC_{0-24 h} was (1 343.46±186.89) ng·h·mL^-1, AUC_0-∞ was (1 351.31±188.79) ng·h·mL^-1. Conclusion: This method is easy to operate, has high specificity, and sensitivity. It has been successfully applied to the pharmacokinetic study of 8 healthy subjects after oral administration of 50 mg vigagliptin tablets on an empty stomach. Therefore, it can be used as a reliable detection method for human pharmacokinetic research and therapeutic drug monitoring.

Objective: To establish a method for simultaneous determination of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, cynarin, galuteolin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C in Shanjujiangya capsules by HPLC and analyze compositional change of Chrysanthemi Flos combined with law of quantity transfer. Methods: The analysis was performed on Waters Symmetry C₁₈ column (250 mm×4.6 mm,5 μm), with mobile phase composed of acetonitrile -0.1% phosphoric acid solution at a flow rate of 1.0 mL·min^-1 in gradient elution mode. The column temperature was 30 ℃ and the detection wavelength was 328 nm. The transfer rates of the above eight components were used as the indexes for quality evaluation to study the quantity value of transfer rule from the decoction piece to the extracting solution. Results: The results showed that the determination of eight components manifested a good linear relationship in the range of mass concentration (r>0.999 9), the average recoveries of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, cynarin, galuteolin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C were 98.3%-101.9%,with RSDs of 0.066%-0.64%. The contents of the above 8 components in 3 samples were 0.257-0.279 mg·g^-1, 0.629-0.650 mg·g^-1, 0.402-0.476 mg·g^-1, 0.454-0.539 mg·g^-1, 1.118-1.278 mg·g^-1, 0.653-0.740 mg·g^-1, 0.659-0.706, 1.138-1.167 mg·g^-1, respectively. Conclusion: The HPLC method established in this study is simple, repeatable and stable. The analysis of quantity transfer provides data support for the establishment of content methods and the formulation of limits. This study can provide basis for quality control method of Shanjujiangya capsules.

Objective: To establish a fingerprint of Gualou Guizhi decoction and a method for determination of multi-component to clarify the transfer rule of quantities and quality from decoction pieces and substance benchmarks. Methods: Fifteen batches of Gualou Guizhi decoction substance benchmarks were prepared and analyzed by the method of HPLC. Traditional Chinese medicine (TCM) Chromatographic Fingerprint Similarity Evaluation Software (2012) and hierarchical cluster analysis (HCA), principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) was used to evaluate the quality differences between batches of substance benchmarks, and screen the main chemical compositions that were led to quality discrepancy. The main differential components were determined by HPLC. And their contents, yields and transfer rates were analyzed for transfer rule of quantities and quality. Results: HPLC fingerprint of Gualou Guizhi decoction was established. A total of 30 common peaks in the fingerprint of Gualou Guizhi decoction substance benchmarks were assigned. Compared with the reference standards, 9 components were identified as gallic acid, albiflorin, paeoniflorin, liquiritin, ononin, liquiritigenin, cinnamic acid, isoliquiritigenin and glycyrrhizic acid. The similarities of 15 batches of Gualou Guizhi decoction substance benchmarks samples were all above 0.920. All of them were divided into two categories by three chemical recognition modes for 5 major differential components, including glycyrrhizic acid, liquiritigenin, paeoniflorin, iquiritin, and ononin. The HPLC was also applied to determine the contents of multi-components and the method validation results were good. The average transfer rates of five index components were 51.65%, 40.46%, 74.74%, 60.06%, and 34.54%, respectively and their average extraction rate was 14.20%. Conclusion: The critical quality properties of Gualou Guizhi decoction can be stably transferred from decoction pieces to substance benchmarks. The method of fingerprint and content determination is accurate and reliable, which is able to provide technique for quality control of Gualou Guizhi decoction formulation.

Objective: To compare the differences of the volatile oil components of Pimpinella thellungiana Wolff extracted with different methods by GC-MS combined with retention index. Methods: Volatile oil of Pimpinella thellungiana Wolff were extracted using steam distillation, salting-out assisted steam distillation and enzymatic hydrolysis-assisted steam distillation. The chemical components of volatile oil extracted by different methods were analyzed by GC-MS combined with retention index, while the relative contents of volatile oil components were calculated by peak area normalization method. Results: Among the three extraction methods, the extraction rate of volatile oil was as follows, enzymatic hydrolysis-assisted steam distillation > salting-out assisted steam distillation ≈ steam distillation method. The most comprehensive types of volatile oil were extracted by salting-out assisted steam distillation, followed by enzymatic hydrolysis-assisted steam distillation, and finally by steam distillation. The main types of the volatile oil components of Pimpinella thellungiana Wolff extracted with different methods were basically unchanged, but the relative contents of various compounds were different. A total of 47 compounds were identified from the volatile oil extracted with the three methods, including 35 common compounds. The main chemical structural types of these compounds were terpenes, terpenes, terpenoids, aromatics and aliphatics, among which the higher content compounds were β-bisabolene(17.25%-19.42%), caryophyllene oxide (12.90%-15.70%), 1-(3-methyl-2-butenoxy)-4-(1-propenyl)benzene (5.02%-9.36%) and β-pinene (5.31%-6.62%). Conclusion: The chemical composition types and relative contents of the volatile oil of Pimpinella thellungiana Wolff extracted with different methods are different, but the differences are not significant. The results can provide reference for the selection of suitable extraction methods and further utilization of volatile oil from Pimpinella thellungiana Wolff.

Objective: To establish a suitable method to determine the structure and source of impurities of colistimethate sodium (CMS) for drug quality control studies. Methods: Frist-dimensional system: using Acquity UPLC^® Peptide CSH C₁₈(150 mm×2.1 mm, 1.7 μm) column, the mobile phase A was phosphate buffer (7.8 g·L^-1 sodium dihydrogen phosphate, adjusted to pH 6.4 with 1 mol·L^-1 sodium hydroxide)- acetonitrile (19∶1), the mobile phase B was phosphate buffer-acetonitrile (1∶1). Gradient elution was performed at a flow rate of 0.3 mL·min^-1. The column temperature was 30 ℃. Second-dimensional system: the Acquity BEH C₁₈ column (50 mm×2.1 mm, 1.7 μm) column was used with ammonium formate(A)-acetonitrile mixture as mobile phase with gradient elution. The flow rate was 0.2 mL·min^-1. The column temperature was 40 ℃. The detection wave length was 210 nm. The ESI source was used in negative ion mode. Results: The 2D-LC-Q TOF MS method was used to infer the structure of the 55 impurities in CMS, and the main sources were polymyxin E1-I, polymyxin E1-7MOA, polymyxin E3 and polymyxin E6. Conclusion: The structure and source of impurities in CMS are determined by 2D-LC-Q TOF MS, and the changes in the content of impurities such as manufacturers and production processes are evaluated, which is conducive to improving the production process and controlling drug quality at the source.

Objective: To comprehensively evaluate the quality of Poriae Cutis, and to establish a dual wavelength switching HPLC method for comparing the characteristic spectra of Poriae Cutis and studying the content of 11 triterpenoid components, to provide reference for the qualitative and quantitative research of Poriae Cutis. Methods: Agilent 5 HC-C₁₈(2) column(250 mm×4.6 mm, 5 μm) was adopted. Acetonitrile solution (contain 3% tetrahydrofuran) (A) and 0.1% formic acid aqueous solution (B) were used as the mobile phase with gradient elution at a flow rate of 1.0 mL·min^-1. The column temperature was 30 ℃ and the injection volume was 20 μL. The detection wavelengths were 210 and 243 nm. Results: The feature profiles developed were effective in identifying the 18 shared peaks. RSD for precision, repeatability and stability (48 h) tests were all less than 3.72%(n=6). The 11 chemical components to be measured were well separated, with good linearity in the mass range examined (all r ≥ 0.999 6). The average recovery rate was 95.4%-105.5%, and the RSD was 1.0%-3.1%. The RSDs of precision, repeatability, and stability (48 h) tests were all less than or equal to 3.0%(n=6). The results of similarity analysis showed that most of the origins of Poriae Cutis were very similar to each other. The results of content determination showed that among the 11 triterpenoid constituents, poricoic acid A accounted for the highest percentage in all batches of Poriae Cutis. In addition, the content of five components, poricoic acid A, dehydrotrametenolic acid, poricoic acid B, dehydroeburicoic acid and trametenolic acid, fluctuated relatively more, while the other components fluctuated more gently. No significant geographic variation in samples from different origins. Conclusion: A method for the determination of Poriae Cutis characteristics and multi-component content was established, which laid the foundation for quality control of Poriae Cutis.

Objective: To establish an HPLC method for the determination of six related substances in N-fluorenylmethoxycarbonyl-O-tert-butyl-L-threonine. Methods: The analysis was conducted on YMC Triart C₁₈(250 mm×4.6 mm, 3μm) column, the mobile phase was consisted with 0.1% trifluoroacetic acid in water(A) and 0.1% trifluoroacetic acid in acetonitrile(B)at the flow rate of 1.0 mL·min^-1. The column temperature was set 30 ℃, the detection wavelength was 265 nm and the injection volume was 10 μL. Results: N-Fluorenylmethoxycarbonyl-O-tert-butyl-L-threonine had good separation from the adjacent impurity peaks; The resolution of impurity1- 6 was greater than 1.5, and showed a good linear relationship (r≥0.999) in the corresponding mass concentration range, the detection limit of impurity 1-6 was 0.03 μg·mL^-1, and the quantitative limit was 0.06 μg·mL^-1, the average recovery rate (n=9) of impurity 1-6 was in the range of 97.6%-98.8%. The results of the three batches of N-fluorenylmethoxycarbonyl-O-tert-butyl-L-threonine showed that the contents of impurity 2, impurity 4 were <0.2% and <0.1%, respectively, and the other four impurities were not detected, and content of the total impurity was <1%. Conclusion: This method has good resolution, high sensitivity and strong specificity, and is suitable for the determination of related substances in N-fluorenylmethoxycarbonyl-O-tert-butyl-L-threonine.

Objective: To establish an ion chromatography method for determination the content of sodium caprylate in human blood albumin products. Methods: The samples were precipitated with eluent, the suspension was centrifuged and filtered, the filtrate was injected to IC, and heptanoic acid was used as the internal standard. A Dionex InPac^TM NS1 Analytical Column (250 mm×4mm, 10 μm) and a Dionex InPac^TM NG1 Guard Column (35 mm×4 mm, 10 μm) were used,the flow rate was 1.0 mL· min^-1. The conductivity detector and ASRS 300 membrane suppressor were used, and the regenerant solution was 5 mmol·L^-1 tetrabutylsodium hydroxide solution;the column temperature was 30 ℃ and the injection volume was 25 μL. Results: The resolution between the peaks of sodium caprylate and the internal standard was greater than 1.5, and the linearity of concentration of sodium caprylate was good in the range of 0.38-2.52 mmol·L^-1, r=0.999 5 (n=6). The RSD of the repeatability test was 1.1% (n=6). The average recovery was 97.4% and RSD was 1.8% (n=9). The limits of quantification and detection were 0.19 nmol and 0.09 nmol, respectively. The determination results of the content of sodium octanoate in 20 batches of human blood albumin samples from 7 enterprises at home and abroad ranged from 0.073-0.163 mmol·g^-1. Conclusion: The method established in this study is simple to operate, accurate in results, high in sensitivity and good in repeatability, can be used for the determination of sodium caprylate content in human blood albumin products and provide a method guarantee for its quality control.

Objective: To establish a method for determination of potential anti-vascular disease active components of Semen raphani based on cell membrane chromatographic (CMC) model of human umbilical vein cell (HUVEC). Methods: The HUVEC cell membrane chromatography coupled with HPLC-ESI IT TOF MS system were used to screen the active components of Semen raphani. The selected active components were further applied to ox-LDL induced HUVEC to verify their protective effects. Results: Two retained components were selected from Semen raphani by this method. One component was identified as erucinic acid by comparing with the reference material. Compared with the model group, the cell survival rates of the erucinic acid pretreatment groups increased significantly. The amount of ICAM-1 and VCAM-1 decreased in a dose-dependent manner. Bcl-2 protein levels decreased and Bax protein levels increased, with statistical significance (P<0.05). Conclusion: The method can rapidly obtain active ingredients from complex traditional Chinese medicines. It provides a reference for the application of cell membrane chromatography and the development of Semen raphani.