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.

Objective: To develop an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of 16 saponins (notoginsenoside R₁, notoginsenoside Fa, notoginsenoside Fe, ginsenoside Re, ginsenoside Rg₁, ginsenoside Rf, ginsenoside F₃, ginsenoside Rg₂, ginsenoside Rb₁, ginsenoside F₁, ginsenoside Rb₂, ginsenoside Rb₃, ginsenoside Rd, ginsenoside F₂, ginsenoside Rg₅, and 20(S)-ginsenoside Rg₃) in compound Sanqi capsules, and to evaluate the quality of these compound Sanqi capsules. Methods: The samples were extracted with methanol using ultrasonic extraction, and separation was performed on a Thermo Fisher Scientific Accucore Phenyl Hexyl column (2.1 mm×100 mm, 2.6 µm) using gradient elution, with 0.1% formic acid aqueous solution (A) and acetonitrile (B) as mobile phase. The flow rate was 0.4 mL · min^-1, the column temperature was 35 ℃, and the injection volume was 2 μL. Mass spectrometry was performed by using a heated electrospray ion source (HESI), and parallel reaction monitoring (PRM) in negative ion mode was employed for data acquisition and determination. The spray voltage was 2.8 kV(-). Results: The established method showed a good linear relationship within a certain concentration range (r≥0.997 0). The precision, repeatability and stability of the tested samples were good with recoveries ranging from 96.6% to 102.3%, and the RSDs between 1.1% and 5.1%. The results indicated that the contents of the 16 saponins were different among samples from different manufacturers and different batches of samples from the same manufacturer. The average total saponin contents of the samples from the three manufacturers were 33 019.650 8, 32 801.840 8, and 27 108.822 0 μg · g^-1 respectively. Among the 10 batches of samples, the one with the lowest content was ginsenoside Rf and the top five saponin components in terms of content were ginsenoside Rg₁, ginsenoside Rb₁, notoginsenoside R₁, ginsenoside Rd, and ginsenoside Re in sequence. Moreover, the average total contents of these five saponins all accounted for more than 95% of the total saponins, and could be used as markers that contribute significantly to quality differences. Additionally, cluster analysis could be divided into 3 categories according to manufacturers. Statistics showed that in the samples classified by cluster analysis as class Ⅰ, the dispersion degrees of the other saponins in the box diagram were greater than thoes in class Ⅱ and class Ⅲ. except ginsenoside Rb₂ and contents of ginsenoside Rg₅ were significantly higher than those in class Ⅱ and class Ⅲ, with a significant difference (P<0.001). The qualities of 3 batches of samples in class Ⅱ were stable, and contents of ginsenoside Rb₂ were significantly different from those in class Ⅰ and class Ⅲ (P<0.001). The components of saponins in class Ⅲ samples were lower than those in class Ⅰ and class Ⅱ samples. Conclusion: The method can quickly, efficiently and accurately determine the contents of 16 saponins in compound Sanqi capsules, and provides a reference for the quality control of compound Sanqi capsules.

Pharmacological studies have demonstrated the important role of flavonoids in promoting human health. The determination of pharmacological activity requires using of monomeric compounds. However, the advancement of precision medicine has imposed more stringent requirements on compounds, especially compounds intended for therapeutic use. In chiral drug research, the impact of optical isomers on drug efficacy should not be overlooked. While most drugs are used in clinical practice as racemates, certain isomers may not only reduce therapeutic efficacy, but increase metabolic load or even cause toxicity. Chiral stationary phases (CSP) are important materials for obtaining optically pure flavonoid compounds and represent a core aspect of chiral research. This review summarizes the recent developments in chiral stationary phases for the enantioseparation of flavonoids, in order to provide a reference for the chiral separation of flavonoids and offer new perspectives for further exploration and utilization of flavonoid compounds.

Objective: To explore the fragmentation patterns of synthetic cannabinoids by electron impact (EI) ionization mass spectrometry. Methods: Forty synthetic cannabinoids were systematically investigated by gas chromatography coupled to mass spectrometry (GC-MS). Ionization mode was EI (70 eV) and the acquisition range was m/z 50-600. Results: According to the different structures of the “head group” and “linked group”, forty synthetic cannabinoids were divided into six categories, namely cumyl-carboxamide type, adamantyl-carboxamide type, carbamoyl/methyl butyrate-carboxamide type, naphthylformyl type, benzoyl/phenylacetyl type and tetramethylcyclopropane-acyl type. Through the analysis of the mass spectrum of synthetic cannabinoids, the fragmentation pathways and characteristic ions of different types of synthetic cannabinoids were given. The main EI-MS fragmentation patterns of synthetic cannabinoids were that both sides of the carbonyl group in the “linking group” undergo α-cleavage, and the N atom on the indole/indazole parent nucleus was prone to γ-H rearrangement, and loss of a R₁. In addition, fragment ions m/z 116, 130, 144 and fragment ions m/z 117, 131, 145 were the characteristic fragments of indazole and indole parent nucleus, which could be used to identify the parent nucleus of synthetic cannabinoids. Conclusion: These kind of compounds have strong fragmentation regularity. When standard substances are lacking or commercial mass spectral libraries are difficult to obtain, the proposed synthetic cannabinoids EI-MS fragmentation pathways can help to rapidly identify the structures of unknown synthetic cannabinoids.

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.

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 analyze the fractions and relative contents of volatile oils of Magnoliae Flos at different harvesting periods, to elucidate the dynamic pattern of changes in the chemical composition of Magnoliae Flos at five harvesting periods, and to evaluate its antioxidant and antimicrobial activities. Methods: The volatile oils of Magnoliae Flos at five harvesting periods was extracted by water vapour distillation, and the chemical composition was analyzed by gas chromatography-mass spectrometry (GC-MS) technique, and the relative content of each constituent was calculated. The constituents of Magnoliae Flos at the five harvesting periods were analyzed by PLS-DA analysis, which was used in combination with the VIP value to screen out the differential compounds. The antioxidant activity of the volatile oil of Magnoliae Flos was determined by ferric ion reducing antioxidant power (FRAP) method, and its in vitro antimicrobial activity was investigated by 96-well plate method. Results: The total volatile oils content of Magnoliae Flos was the highest in samples at the 4th harvesting period (10 February 2023). Thirty-eight components were identified in the volatile oils of Magnoliae Flos, and 12 differential compounds were screened, including γ-muurolene, elemene, δ-cadinene and α-terpineol, etc. The relative contents of γ-muurolene, alloaeromadendrene, borneol, camphor and cis-4-thujanol were the largest in samples at the 4th harvesting period, which was basically in line with the trend of the change of volatile oil content. The volatile oils in samples at five harvesting period showed certain antioxidant and antibacterial activities. And that in samples at the 4th harvesting period showed the strongest antioxidant activity and the inhibition ability against all five species of bacteria. Conclusion: The chemical composition of the volatile oils in Magnoliae Flos was basically the same in in samples at five harvesting periods, but there is a significant difference in the relative content of its volatile components in each harvesting period, and it is presumed that the beginning of February is the optimal harvesting period for Magnoliae Flos.

As one crucial resource of Chinese medicines, fungal Chinese medicine have been extensively used in clinic. This article has compiled a total of 442 standards for fungal Chinese medicine that have been issued in China, including 19 Chinese Pharmacopoeia standards, 398 local standards and 25 bureau or ministry standards. The fungal Chinese medicine are composed by 67 traditional Chinese medicine varieties from 66 fungal species. Based on the review of those quality standards, the characteristics and quality evaluation of fungal Chinese medicine such as medicinal property, microscope appearance, DNA based identification and physicochemical identification, assay (polysaccharides, nucleosides, sterols, terpenes, proteins/peptides, esters, sugar alcohols, etc.), microbial and harmful substances, as well as related analytical techniques are summarized. This review will certainly provide the comprehensive understanding of current research and development of fungal Chinese medicinal materials.