OBJECTIVE To compare technical documents on criteria for chromatographic-mass spectrometric confirmation of the identification of analytes in major international organizations,and provide suggestion for updates of corresponding technical specifications in Chinese Pharmacopeia. METHODS Chinese Pharmacopeia volume Ⅳ,the guidance or technical documents in European Commission,Food and Drug Administration,and World Anti-Doping Agency were reviewed.The key parameters in relevant technical documents were compared. RESULTS The criteria in different organizations were updated following the repaid development of analytical techniques.Existing technical documents also vary in their requirements for specific technical parameters. CONCLUSION It is suggested that the criteria for chromatographic-mass spectrometric confirmation of the identification of analytes in Chinese Pharmacopeia general chapter 0431 mass spectrometry should be specified to provide more detailed guidance and ensure relevant methods executed scientifically and standardly.

OBJECTIVE To prepare a new type of hyaluronic acid-decenylsuccinic anhydride (HA-DSA) nanomicelles loaded with plumbagin (PLB),and to study their quality and in vitro drug release. METHODS Firstly,the drug-loaded material HA-DSA was synthesized, and then the formulation process of PLB-HA-DSA was optimized by Box-Behnken response surface and the in vitro release of PLB-HA-DSA was evaluated by dialysis method and the optimal equation was fitted. RESULTS The optimal formulation process of PLB-HA-DSA was as follows: organic phase-aqueous phase(1∶20),drug:material ratio(1∶11). PLB-HA-DSA was spherical with a particle size of (110.71±2.03) nm, a Zeta potential of (-42.12±2.34) mV,an encapsulation efficiency of (92.12±0.06)%, and a drug load of (5.68±0.06)%. In the in vitro release experiment,the cumulative release degree of PLB-HA-DSA was significantly lower than that of the API. CONCLUSION PLB-HA-DSA nanomicelles are successfully prepared, which could retard the release of PLB in vitro and have a certain sustained release effect.

OBJECTIVE To study the chemical composition of Gukang Capsules by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitwell high resolution mass spectrometry(UPLC-QE-Orbitrap-MS/MS).METHODS The analysis of 70%methanol extract of the drug was performed on a 45 ℃ thermostatic Hypersil GOLD C₁₈ column(2.1 mm×100 mm,1.9 μm)with mobile phase consisting of 0.1%formic acid solution-acetonitrile gradiently eluted at 0.3 mL·min^-1,and the injection volume was 1 μL.The information of the chemical constituents of Gukang Capsules was acquired in positive and negative ion modes by electrospray ion source,and the chemical composition was analyzed and identified by software combined with control comparison,database matching,literature reports and mass spectrometry rules. RESULTS A total of 137 compounds were identified from Gukang Capsules,mainly including flavonoids,saponins,organic acids and coumarins,etc.,among which 27 compounds were identified by comparison with reference substances and their origins of medicinal materials were determined.CONCLUSION In this study,the main chemical composition of Gukang Capsules was identified by this rapid and efficient analytic method,which laid a foundation for further research on pharmacodynamic substance base and quality control.

OBJECTIVE To investigate the components and characteristic chromatograms of natural myrrh and colloidal myrrh from different origins using gas chromatography-mass spectrometry(GC-MS).METHODS Based on the study of molecular identification techniques for determining the botanical origins of myrrh, GC-MS was utilized to conduct a qualitative analysis of the volatile oil components in 10 batches of colloidal myrrh and 15 batches of natural myrrh. Furthermore, the Traditional Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System was used to establish the characteristic chromatograms for natural myrrh and colloidal myrrh,respectively.The similarity between different origins and the same commercial type of myrrh with their common mode chromatograms was evaluated. RESULTS Natural myrrh contained significantly more volatile components than colloidal myrrh. Colloidal myrrh primarily consisted of low-boiling-point components,whereas natural myrrh contained both low-and high-boiling-point components.The main components of the volatile oils in both types of myrrh were sesquiterpenes. CONCLUSION There are notable differences in the characteristic chromatograms between natural myrrh and colloidal myrrh. However,there are no significant differences in the volatile components between myrrh of the same commercial type but different botanical origins. There are significant differences in the volatile components between natural myrrh and colloidal myrrh.The volatile components of myrrh are related to its commercial type but not to its botanical origin.

OBJECTIVE To study the chemical constituents of different polar parts of Allii macrostemonis Bulbus. METHODS The chemical constituents in Allii macrostemonis Bulbus were isolated and purified by extraction, silica gel column chromatography, reversed-phase silica (ODS) column chromatography, and semi-preparative high-performance liquid chromatography. The compounds were structurally characterized by high-resolution electrospray ionization mass spectrometry and nuclear magnetic resonance spectrometry (NMR). Meanwhile, the antioxidant activity of each of the compound was determined in vitro using the 2,2-diphenyl-1-picrylhydrazyl free radical (DPPH·) and the 2,2'-amino-bis(3-ethyl-benzothiazoline sulfonate-6) ammonium salt radical (ABTS·) scavenging method. RESULTS Twenty-four compounds were isolated from Allii macrostemonis Bulbus. Two compounds were isolated from the petroleum ether fraction and identified as oleic acid (1) and dodecanoic acid (2). Five compounds were isolated from the dichloromethane fraction and identified as kaempferol (3), isorhamnetin (4), oleanolic acid (5), sarsasapogenin (6), and tigogenin (7). Sixteen compounds were isolated from the n-butanol fraction and identified as (+)-catechin (8), quercetin (9), harpagide (10), magnoflorine (11), synephrine (12), gallic acid (13), syringin (14), thymidine (15), guanosine (16), β-sitosterol (17), stigmasterol (18), daucosterol (19), dibutyl phthalate (20), L-tryptophan (21), respectively, 7,7'-bis-(4-hydroxy-3,5-dimethoxyphenyl)-8,8'-dihydroxymethyl-tetrahydrofuran-4-O-β-D-glucopyranoside (22), and polianthoside B (23). One compound, betaine (24), was isolated from the aqueous fraction. The in vitro antioxidant results showed that compound 9 had the strongest scavenging ability for DPPH· and ABTS·, with IC₅₀ values of (0.32±0.11) mg·mL^-1 and (0.03±0.02) mg·mL^-1, respectively. CONCLUSION Compounds 2-5, 8-12, 20 and 22-24 are isolated from this plant for the first time, with compounds 22 and 23 being isolated for the first time from Liliaceae family.

OBJECTIVE To analyze the results of three NMPA's Microbial Proficiency Testing Programs, NIFDC-PT-288, NIFDC-PT-340, and NIFDC-PT-446, to evaluate the microbiological testing abilities of laboratories nationwide in drug detection, thus the regulatory agencies can learn the microbiological proficiency status of drug inspection laboratories and the laboratories can improve the microbiological detection ability. METHODS The results of the three proficiency testing programs were analyzed regarding the satisfaction rate, identified problems, and key technical points, and the laboratory types, number of laboratories and capability of the laboratories participating the three proficiency testing projects were analyzed. RESULTS The result satisfaction rates of provincial food and drug inspection institutions were 95.7% (NIFDC-PT-288), 86.4% (NIFDC-PT-340) and 100.0% (NIFDC-PT-446), while the satisfaction rates of municipal food and drug control institutions were 95.5% (NIFDC-PT-288), 83.9% (NIFDC-PT-340) and 92.5% (NIFDC-PT-446), respectively. The satisfaction rates of enterprise laboratory were 86.7% (NIFDC-PT-288), 65.7% (NIFDC-PT-340) and 80.2% (NIFDC-PT-446), respectively. The satisfaction rates of other types of laboratories were 100.0% (NIFDC-PT-288), 61.5% (NIFDC-PT-340) and 86.7% (NIFDC-PT-446), respectively. CONCLUSION The successful implementation of the three microbiological proficiency testing programs has provided the laboratories with effective external quality control means, and it also provides the first-hand reference for regulatory authorities on the microbiological testing capability of nationwide drug laboratories. The qualitative microorganism testing ability of drug laboratories is basically good, while the quantitative microorganism testing ability needs to be improved.

OBJECTIVE To establish a method for the quantitative detection of bacterial endotoxin in glutamic acid and verify its feasibility. METHODS Verification test of the reliability of bacterial endotoxin standard curve, interference test of calcium ion buffer and sodium ammonium hydrogen phosphate used in pre-treatment, and interference test of test product and additional endotoxin recovery test were carried out in sequence by using limulus reagents from two manufacturers according to the standard of kinetic chromogenic assay in bacterial endotoxin inspection method (General Chapter 1143 in Chinese Pharmacopoeia2020 Edition). A method for the detection of bacterial endotoxin in glutamic acid was successfully established, and three batches of samples were quantitatively detected by this method. RESULTS Glutamic acid was dissolved with sodium ammonium hydrogen phosphate together to the concentration of 20 mg·mL^-1, then diluted by calcium ion buffer to the concentration of 5 mg·mL^-1, which had no interference effects on bacterial endotoxin test. The contents of endotoxin in three batches of samples were all lower than the limit of 12 EU·g^-1, the RSD values were all lower than 10%, and the endotoxin recovery rates were in the range of 50% to 200%, which met the requirements. CONCLUSION The bacterial endotoxin test method established in this study can be used to detect the bacterial endotoxin in glutamic acid and control its quality.

The concept of entropy is originated from physics which represents a degree of disorder. Entropy increase is a natural law for extinction of things. In the field of life science, entropy could be used to measure the quality of life. Organisms utilize their inherent negative entropy mechanisms of self-organization, defense, self-healing, wear resistance, and adaptability to counteract entropy increase, and thus to cure various diseases and curb aging processes, while maintaining optimal health. As an external intervention, good drugs could trigger negative entropy mechanisms by enhancing one or more of the above machineries, thus assist the body to recover. This article explores the potential applications of biological entropy in drug discovery research, aiming to leverage its power in the future for a good understanding of drug targets, elucidation of drug mechanisms, rational design of novel drugs and rigorous evaluation of drug efficacy, especially pertinent to multi-target drugs.

OBJECTIVE To explore the supercritical CO₂ extraction process of Curcuma longa L. and its effects on alleviating alcohol intoxication and protecting the liver. METHODS The extraction yield, curcumin, and α-turmerone contents were used as evaluation indicator. Single-factor experiments and orthogonal experimental designs were employed to optimize process parameters such as the amount of co-solvent, extraction pressure, extraction temperature, extraction time, separation vessel pressure, and temperature. The alcohol alleviating effects, pathways, and liver protection of Curcuma longa L. Supercritical CO₂ extract were evaluated using mouse alcohol intoxication models, rat alcohol intoxication models, and mouse subacute alcohol-induced liver injury models. The results indicated that the optimal process for Curcuma longa L. RESULTS Supercritical CO₂ extraction included: an extraction pressure of 30 MPa, extraction temperature of 55 ℃, using ethanol as a co-solvent at a weight equal to that of the medicinal material, an extraction time of 2 hours, maintaining consistent pressure in the separation vessel and storage tank, a separation vessel temperature of 40 ℃, and ethanol recovery through depressurization at 50 ℃. Furthermore, the supercritical extract significantly reduced the sleep time of mice after alcohol intoxication and improved their wake-up experiment (P<0.01), increased the ADH level in rats (P<0.01), and reduced the levels of TC, LDL-C, and TBIL in the serum of mice in the subacute liver injury model (P<0.01). CONCLUSION The preparation process developed in this study has a high extraction rate, is stable and feasible, and the supercritical CO₂ extract produced exhibited good alcohol alleviating effects and reduces subacute alcohol-induced liver injury.

OBJECTIVE To establish an inductively coupled plasma mass spectrometry (ICP-MS) method for the simultaneous determination of 22 kinds inorganic elements in Broussonetia papyrifera leaves, analyze the differences of inorganic elements in leaves from different origins, and evaluate the safety and health risks of heavy metals and harmful elements, so as to provide a reference for the quality evaluation of Broussonetia papyrifera leaves and the effective development of resources. METHODS After microwave digestion of Broussonetia papyrifera leaves, 22 elements were analyzed by ICP-MS using Relative molecular mass similar elements as internal standards. After methodological investigations, samples were analyzed, and the orthogonal partial least squares discriminant analysis (OPLS-DA) method was utilized to compare variability of inorganic elements from diverse sources. Safety was evaluated by individual pollution index(Pi) and comprehensive pollution index(Pc), while health risk was assessed by calculating maximum daily intake of heavy metals (EDI), target hazard quotient (THQ), and carcinogenic risk (CR). RESULTS The linearity of the 22 elements determined was excellent with a correlation coefficient r²≥0.991. The relative standard deviation (RSD) values of precision, stability, and reproducibility tests met analytical requirements. The detection limit of each element was between 0.000 6 to 1.687 3 μg·L^-1, and recovery rate was between 83.63% and 106.58%. The contents of K, Ca, Mg, and P in 24 batches of leaf samples from different origin were higher, which were 19 098, 5 258, 4 882 and 2 904 mg·kg^-1, respectively. Principal component analysis revealed 5 key factors, identifying Co, Al, Fe, Ni, Sr, Mg, and K as the main characteristic elements of Broussonetia papyrifera leaves. Pi and Pc had excellent safety ratings. EDI and CR results indicated no potential health risks from heavy metals and harmful elements in Broussonetia papyrifera leaves, but THQ suggests that the as element in the leaves may have an impact on human health. CONCLUSION The Broussonetia papyrifera leaves are rich in inorganic elements, heavy metals and harmful elements have less impact on human health, the content of essential elements such as K, Ca, Mg, Fe, Na and Zn are high. This method is sensitive, rapid and accurate for the quantitative analysis of the inorganic elements in Broussonetia papyrifera leaves, which has important value for the study of its inorganic elements.