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.

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.

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.

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.

To establish an HPLC method for simultaneous determination of seven components(narirutin, naringin, hesperidin, neohesperidin, naringenin, nobiletin and atractylenolide Ⅲ) in Zhizhu granules. And to provide reference for its quality evaluation by using chemometric analysis.

The chromatographic column Waters Symmetry C₁₈(250 mm×4.6 mm，5 μm) was adopted using HPLC-DAD. The mobile phase consisted of acetonitrile (A)-0.1% phosphoric acid (B) in gradient elution with flow rate of 1.0 mL·min^-1, the detection wavelength were 220 nm (atractylenolide Ⅲ), 280 nm (narirutin, naringin, hesperidin, neohesperidin and naringenin) and 332 nm (nobiletin). The column temperature was set at 30℃ and the injection volume was 10 μL. Cluster analysis, principal component analysis and orthogonal partial least squares-discrimination analysis were used to distinguish the content determination results.

The resolution of each component in 24 batches of Zhizhu granules was good, and the linear relationship between concentration and peak area was good (r>0.999 9). The average recoveries were within 87.6%-114.3%. There were some differences in 24 batches of Zhizhu granules, and 4 different components were screened out, which were naringin, hesperidin, neohesperidin and naringin. The contents of narirutin, naringin, hesperidin, neohesperidin, naringenin, nobiletin and atractylenolide Ⅲ in 24 batches of Zhizhu granules samples were 0.378 4-1.380 1 mg·g^-1, 5.125 8-18.137 6 mg·g^-1, 0.283 9-1.195 8 mg·g^-1, 4.490 3-22.585 0 mg·g^-1, 0.022 5-0.349 8 mg·g^-1, 0.063 3-0.211 4 mg·g^-1 and 0.054 7-0.137 5 mg·g^-1, respectively.

The established method is accurate, reliable and reproducible, which can provide reference for the quality control of Zhizhu granules.

To establish a method of UPLC fingerprint and quantitative analysis of gallic acid, protocatechuic acid, p-hydroxycinnamic acid, myricitrin and quercitrin for Frucius Aceris Fabri, and to provide a reference for the quality control of Frucius Aceris Fabri.

The determination was performed on a Waters CORTECS UPLC T3 column (150 mm×2.1 mm, 1.6 μm), with mobile phase consisting of acetonitrile -0.1% phosphoric acid by gradually elution at a flow rate of 0.20 mL·min^-1. The column temperature was 30 ℃, and detection wavelength was set at 300 nm. The quality of 10 batches of Frucius Aceris Fabri was evaluated by similarity analysis, CA and TOPSIS analysis of fingerprints.

The UPLC fingerprint of Frucius Aceris Fabri was established, and 14 peaks were selected as the characteristic fingerprint peaks. Five chemical components were identified, which were gallic acid, protocatechuic acid, p-hydroxycinnamic acid, myricitrin and quercitrin. And a quantitative method for the determination of the 5 chemical components was established. Good similarities were found in the established fingerprint through similarity analysis. CA and TOPSIS analysis showed that 10 batches of Frucius Aceris Fabri samples could be clustered into 3 groups. The sample S9 from Jiangxi was classified as class Ⅰ with best quality. The samples from Guangxi and Guangdong were classified as Class Ⅱ with medium quality. The samples S1, S4 and S6 from Jiangxi were classified as Ⅲ with worst quality. The linear relationship of the 5 chemical components was good, and the r values were all above 0.999. The contents of the 5 chemical components in 10 batches of samples were 0.236-0.356 mg·g^-1, 0.118-0.398 mg·g^-1, 0.108-0.141 mg·g^-1, 0.146-0.222 mg·g^-1 and 0.046-0.104 mg·g^-1, respectively.

The established UPLC fingerprint and quantitative analysis methods of Frucius Aceris Fabri are precise and stable, which can be used for evaluating and controlling the quality of Frucius Aceris Fabri.

To establish an HPLC method for simultaneous determination of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, forsythiaside A, 3，4-O-dicaffeoylquinic acid, 3，5-O-dicaffeoylquinic acid, 4，5-O-dicaffeoylquinic acid, forsythin, andrographalide and dehydroandrographalide in compound Shuanghua tablets.

The samples were extracted with 50% methanol solution under ultrasonic condition, and were performed on Agilent Zoabax SB-C₁₈ column (250 mm×4.6 mm, 5 μm) by gradient elution of acetonitrile -0.15% phosphoric acid solution at a flow rate of 1.0 mL·min^-1. The column temperature was 30 ℃, the injection volume was 10 μL, and the detection wavelength were set at 327 nm (detecting neochlorogenic acid，chlorogenic acid, cryptochlorogenic acid, forsythiaside A，3，4-O-dicaffeoylquinic acid，3，5-O-dicaffeoylquinic acid and 4，5-O-dicaffeoylquinic acid) and 226 nm (detecting forsythin, andrographalide and dehydroandrographalide).

The linear ranges of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid，forsythiaside A，3，4-O-dicaffeoylquinic acid, 3，5-O-dicaffeoylquinic acid, 4，5-O-dicaffeoylquinic acid, forsythin, andrographalide and dehydroandrographalide were 4.071-40.71 μg·mL^-1(r=0.999 9), 20.16-201.6 μg·mL^-1(r=0.999 9), 4.730-47.30 μg·mL^-1(r=0.999 9), 4.536-45.36 μg·mL^-1(r=0.999 8), 1.817-18.17 μg·mL^-1(r=0.999 9), 2.266-22.66 μg·mL^-1(r=0.999 7), 3.321-33.21 μg·mL^-1(r=0.999 9), 3.462-34.62 μg·mL^-1(r=0.999 6), 2.111-21.11 μg·mL^-1(r=0.999 9) and 2.290-22.90 μg·mL^-1(r=0.999 7), respectively. The average recoveries (n=6) were 101.3%(2.1%)，103.0%(1.5%)，100.9%(2.0%)，101.1%(2.0%)，98.4%(1.6%)，102.2%(2.4%)，98.2%(1.3%)，97.8%(2.0%)，99.0%(2.0%) and 96.4%(1.1%), respectively. The contents of the 10 components in 4 bacthes of Fufang Shuanghua tablets were in the range of 1.685-2.649 mg·g^-1, 12.202-13.780 mg·g^-1, 2.415-2.594 mg·g^-1, 1.340-1.919 mg·g^-1, 0.501-0.791 mg·g^-1, 0.891-1.342 mg·g^-1, 1.299-2.105 mg·g^-1, 1.147-1.504 mg·g^-1, 0.654-0.694 mg·g^-1, 0.846-1.151 mg·g^-1, respectively.

This simple accurate reproducible method can be used for the quality control and evaluate of compound Shuanghua tablets.

To establish an ion chromatography method for determination the content of sodium caprylate in human blood albumin products.

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.

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.

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.

To establish a method for determining molecular weight and distribution of raw mannatide and its preparation with SEC-RI-MALLS.

Specificity，accuracy, precision and robustness of SEC-RI-MALLS method was verified by performing on a Shodex OHpak SB-804 HQ column with 0.05 mol·L^-1 sodium sulfate buffer as mobile phase at a flow rate of 0.5 mL·min^-1 and a comparison between SEC-RI-MALLS and GPC was studied too.

The tablet excipient starch had no interference to the test. The relative accuracy error between the measured value and the labeled value of dextran standard was less than 3.0%. RSD of precision was 0.40% when the sample concentration was 2 mg·mL^-1 and the RSD of reproducibility and robustness were less than 5.0%. There was no significant difference between Shodex OHpak SB-804 HQ column and TSK-GEL G4000 PW_XL column by comparing the results of 79 batches of samples. Compared with the national standard method (GPC) for molecular weight determination, the molecular weight of SEC-RI-MALLS method was 19 509 Da higher on average, and the molecular weight distribution was more concentrated.

SEC-RI-MALLS method can determine the molecular weight and distribution of mannatide without standard with good accuracy and robustness. Compared with the existing method, SEC-RI-MALLS method is more conducive to the safety and effectiveness control of the variety.

To establish a bridging enzyme-linked immunosorbent assay (ELISA) method for the determination of anti-drug antibody(ADA) and a competitive ELISA method for the determination of neutralizing antibody(NAb) in cynomolgus monkey serum, and to conduct methodological validation.

The steps of bridging ELISA method were as follows: the 96-well plates were precoated with telitacicept(RC18) which could combine with anti-RC18 antibody in the samples to form a complex, then were sequentially added biotinylated RC18(Biotin-RC18), horseradish peroxidase conjugated streptavidin (SA-HRP), and tetramethylbenzidine (TMB) substrate solution for color development. After terminating the reaction, the absorbance was read at a wavelength of 450 nm/630 nm on an ELISA reader. The procedures of competitive ELISA method were as follows: the 96-well plates were precoated with B-cell activation factor of the TNF family (BAFF) or a proliferation inducing ligand (APRIL) protein and then were added the samples which was pre-mixed with Biotin-RC18 to form BAFF or APRIL anti-RC18-antibody and Biotin-RC18 complex. SA-HRP and TMB substrate solution for color development were added sequentially. After terminating the reaction, the absorbance was read at an ELISA reader with dual wave length.

The precision of linear range of bridging ELISA method was less than 12.32%, the sensitivity was 50 ng·mL^-1, the critical threshold of screening was 0.937, and the critical threshold of confirmation was 23.62%. The precision of the linear range of competitive ELISA method was less than 20%, the sensitivity was 312.50 ng·mL^-1, and the threshold for determining the activity of NAb against the target BAFF and APRIL was 0.79 and 0.69, respectively. On BAFF and the method of research targets respectively can tolerate 2.5 μg·mL^-1 and 5 μg·mL^-1 RC18 in serum.

The results of method validation indicate that both bridging ELISA and competitive ELISA meet the requirements of preclinical immunogenicity studies of biological products, and can be used for analysis of the concentrations of ADA and NAb in cynomolgus monkey serum.

To compare the in vitro bioactivity between a generic lactobacillin granules drug and three commercial lactobacillin granules drugs, this study investigated inhibition on pathogenic bacteria, the growth promoting effect on probiotics, and establish a method to evaluate the in vitro bioactivity consistency of drugs that regulate gut microbiota.

Two culture systems were set up to investigate the inhibitory effect on pathogenic bacteria and the growth promoting effect on probiotics by lactobacillin granules. The in vitro bioactivity consistency of four products was evaluated by microbial growth curve and analyzed by two-way analysis of variance with Dunnett-t test.

No significant difference (P>0.05) was observed on inhibition of Staphylococcus aureus and growth promotion of Lactobacillus rhamnosus between the generic lactobacillin granules and the commercial lactobacillin granules.

This method could be used to evaluate the in vitro bioactivity of drugs that regulate gut microbiota, and provided guidance on relevant drug development and quality evaluation.

To establish an inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of 25 potentially risky elemental impurities in alfentanil hydrochloride injection.

The Agilent 7800 ICP-MS inductively coupled plasma mass spectrometer was used, the conventional tuning mode was used, the RF power was 1 550 W, the plasma gas flow rate was 15 L·min^-1, the matrix effect was eliminated by external standard, and the sample was diluted for direct injection.

The method can simultaneously determine the content of 25 kinds of elemental impurities, and its linear relationship was good (r >0.99). The RSD of the repeatability test was ≤10% (n=6), and the recovery rate was 80.0%-120.0% (n=9), all of which met the requirements of methodological validation.

The content of elemental impurities in alfentanil hydrochloride injection is lower than 30% of the limit specified in ICH·Q3D, which will not bring safety risks to the drug, providing a reference for the quality control and risk assessment of elemental impurities in other similar drugs.

To establish an HPLC method for the determination of potentially genotoxic impurity E, impurity I, and 2-chloromethyl-4-methoxy-3，5-dimethlpyridine in esomeprazole sodium.

The chromatographic conditions were as follows: impurity E, YMC-Triart C₁₈ column (250 mm×4.6 mm, 5 μm), mobile phase A 0.05 mol·L^-1 monopotassium phosphate buffer, mobile phase B was acetonitrile, the gradient elution program was used at the flow rate of 1.0 mL·min^-1, the detection wavelength was 302 nm and the column temperature was 30 ℃. Impurities I, Agilent Microspher C₁₈ column (100 mm×4.6 mm, 3 μm), mobile phase A was water-phosphate buffer (pH 7.6)-acetonitrile(80∶10∶10), mobile phase B was acetonitrile-phosphate buffer (pH 7.6)-water (80∶1∶19), the flow rate was 1.0 mL·min^-1, the detection wavelength was 302 nm and the column temperature was 30 ℃. 2-chloromethyl-4-methoxy-3，5-dimethlpyridine, GL Inertsil ODS-3 column (250 mm×4.6 mm, 5 μm), mobile phase A was 0.01 mol·L^-1 disodium phosphate solution (pH 6.5), mobile phase B was acetonitrile, the flow rate was 1.0 mL·min^-1, the detection wavelength was 265 nm and the column temperature was 30 ℃.

The linear ranges of impurity E, impurity I and 2-chloromethyl-4-methoxy-3，5-dimethlpyridine were 0.025 1-0.200 7, 0.020 2-0.302 7, 0.126 6-2.110 0 μg·mL^-1. The LOQ of impurity E, impurity I, 2-chloromethyl-4-methoxy-3，5-dimethlpyridine were 0.50, 0.40, 2.53 ng, and the LOD were 0.15, 0.12, 0.84 ng. The average recovery rate ranged from 96% to 104%, and the RSD was less than 2%. No potential toxic impurities were detected in the samples.

The method has the advantages of good repeatability, high precision, high accuracy and good linearity, and the analysis method are simple and efficient.

To establish and verify the helium mass spectrometry detection method to test the sealing integrity of the container closure system (CCS) of pressurized metered dose aerosols (pMDIs).

Determined the maximum allowable leakage limit (MALL) of pMDIs of CCS in the whole life cycle. The special test chambers and helium filling devices were designed and manufactured, and helium filling devices to test the negative and positive control samples under high pressure (absolute pressure 672 kPa) and normal pressure (absolute pressure 100 kPa) respectively. According to the requirements of methodology validation, the validation of detection limit, system suitability, precision, specificity and detection range indicators were completed.The accelerated sample sealing integrity testing for 3, 6 months and 3, 12, 24 months in the long-term stability inspection period was achieved.

Under both helium-filled pressure conditions, the methodological validation indicators were in line with the acceptable standards, and the results of the stability samples were less than the detection limits. This method can detect 100% that the equivalent pore diameter of pMDIs product CCS was 0.095 μm and above.

The helium mass spectrometry detection method can quickly and quantitatively investigate the leakage rate of pMDIs products, prove the seal integrity of CCS with high sensitivity, and meet the industry’s requirements for pMDIs product quality control.

To establish a high-performance liquid chromatography (HPLC) method for investigating the extraction of common antioxidants and extractable sulfur in medical rubber stoppers and the migration of antioxidants and extractable sulfur to propofol medium/long chain fat emulsion injection.

Waters Symmetry RP₁₈(250 mm×4.6 mm，5 μm) was used as chromatographic column with methanol-acetonitrile -1% acetic acid solution as the mobile phase. Detection wavelength, velocity of flow and column temperature were set to 277 nm, 1 mL·min^-1 and 35 ℃.

Good resolution and linear relationship (r≥0.999 6) in the range of 0.1-20 μg·mL^-1 were achieved. This method possesses superior precision, stability, repeatability, and all RSD were less than 5%. The rate of recovery was 93.3%-108.7%, and the RSD was 1.8%-12.5%. The migration of antioxidant BHT was detected in three batches of solution and the content was higher than its corresponding permitted daily exposure (PDE) value, which means there is a large safetyrisk.

The method represents high sensitivity and is easy to operate, which can effectively detect the migration of antioxidants in propofol medium/long chain fat emulsion injection.

To develop an inductively coupled plasma mass spectrometry (ICP-MS) matrix matching method for determination of migration of 11 elements in ketorolac tromethamine injection, including Al, As, B, Ca, Cd, Fe, Mn, Pb, Sb, Si, Ti.

Samples were diluted and capacitated with 1% nitric acid after precipitation with nitric acid. 2% ethanol was added into the standard solution as the matrix. The matrix effect was eliminated by the matrix matching method, and the polyatomic ion interferences were eliminated by the hydrogen collision reaction mode and the helium collision mode.

The linearity of 11 elements was good (r≥0.997 0). The limits of detection were 0. 049-133 ng·mL^-1. The average recoveries of all 11 elements were in the range of 83.8%-107.1%, and the RSD of repeatability was 2.6%-11.0%. Three batches of ketorolac tromethamine injection under acceleration were tested. The overall safety risk was low.

The established matrix matching ICP-MS method is simple, rapid and accurate. It can effectively eliminate the matrix effect and be used for the determination of eleven elemental impurities in ketorolac tromethamine injection, providing technical reference for risk assessment of drug packaging material compatibility.

To determine the polysaccharide hydrolysates from Polygonati Rhizoma under glycoside enzymatic hydrolysis’ HPLC fingerprint. Examine the variations among the polysaccharides produced by the various varieties of Polygonati Rhizoma and provide references for the assessment of the polysaccharide quality.

After the polysaccharide from Polygonati Rhizoma was hydrolyzed by fructose enzymes, its fingerprint was established by HPLC-ELSD. The fingerprint was then analyzed using similarity analysis (SA), hierarchical cluster analysis (HCA), and principal component analysis (PCA) to determine the differences between the polysaccharides from various Polygonati Rhizoma varieties.

Polysaccharides from various strains of Polygonati Rhizoma had different HPLC-ELSD fingerprints, and a total of 17 distinct oligosaccharide fragments were discovered, all of which contained fructose, glucose, and sucrose. Analysis revealed that there are significant intra species differences, minor differences, and high levels of similarity between the three types of Polygonati Rhizoma. The real Polygonati Rhizoma differs significantly from the imitation in several important ways.

Polygonati Rhizoma can be successfully classified according to varieties, using the fingerprint of polysaccharide hydrolysates of the various varieties of Polygonati Rhizoma and its adulterants. The developed HPLC method can be used for the differential analysis of polysaccharides in Polygonati Rhizoma and is straightforward, precise, and repeatable.

To study the preparation and quality control of 3,5-dihydroxy-7,4’-dimethoxyflavone candidate chemical reference substance from Zhuang medicine Amomum paratsaoko S. Q. Tong & Y. M. Xia.

3,5-dihydroxy-7,4’-dimethoxyflavone was separated and purified consecutively by silica gel, recrystallization as well as preparative HPLC. The structure of 3,5-dihydroxy-7,4’-dimethoxyflavone was identified by IR, UV, NMR and other comprehensive spectrum analytical methods with MS spectrum. Its purity was determined by HPLC and TLC, the ash content was determined by incandescent residue method, and the content of 3,5-dihydroxy-7,4’-dimethoxyflavone was calculated by mass balance method. The method for quality analysis of 3,5-dihydroxy-7,4’-dimethoxyflavone candidate reference materials was investigated by HPLC.

The mean value determined by HPLC of 3,5-dihydroxy-7,4’-dimethoxyflavone was 98.85%, the ash value was 0.02%, and the content of 3,5-dihydroxy-7,4’-dimethoxyflavone calculated by mass balance method was 99.83%. The established analytical method was specific and precise.

3,5-Dihydroxy-7,4’-dimethoxyflavone which was prepared in this study met the quality standard requirements of chemical reference substance, and could be used as a reference substance for quality control of medicinal materials and their preparations such as Amomum paratsaoko S. Q. Tong & Y. M. Xia and others. The analysis method was accurate and reliable, which provided a scientific basis for the research and formulation of quality standard of this reference substance.

To evaluate the quality of honeyed Eriobotryae Folium from different habitats and to select the best habitat of honeyed Eriobotryae Folium preferentially based on high performance liquid chromatography fingerprinting and chemical pattern recognition methods.

The detection was performed on an Acclaim^TM 120A C₁₈ (250 mm×4.6 mm, 5 μm) column with the mobile phase of 0.2% aqueous phosphoric acid (A)-acetonitrile (B) in gradient elution (0-5 min, 5%B; 5-6 min, 5%B→10%B; 6-20 min, 10%B; 20-50 min, 10%B→25%B; 50-60 min, 25%B). The volume flow rate was 1.0 mL·min^-1, the detection wavelength was 327 nm, the column temperature was 30 ℃, and the injection volume was 10 μL. The fingerprint profiles of 30 batches of honeyed Eriobotryae Folium from different habitats were established, and the fingerprint profiles combined with chemical pattern recognition were used to conduct comprehensive analysis of honeyed Eriobotryae Folium from different habitats. And cluster analysis(CA), principal component analysis (PCA) and comprehensive scoring were performed on honeyed Eriobotryae Folium from different habitats. Orthogonal partial least squares-discriminant analysis(OPLS-DA) was used to screen out the differential markers of honeyed Eriobotryae Folium from different habitats, and the habitats of honeyed Eriobotryae Folium were selected based on the comprehensive scoring.

The fingerprint profiles of 30 batches of honeyed Eriobotryae Folium were established. Twelve common peaks were identified, and 4 peaks were identified as neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid and auriculoside according to the control finger. CA divided the 30 batches of Honeyed Eriobotryae Folium samples into 6 categories. By PCA, 3 principal components were extracted, with a cumulative variance contribution of 84.315%. Six differential markers were obtained according to OPLS-DA, two of which were identified as chrysoside and chlorogenic acid. The better habitats of honeyed Eriobotryae Folium were screened as Sichuan, Guangxi, Guangdong and Shaanxi according to the comprehensive score.

Good precision, repeatability and stability results are obtained for fingerprinting and content determination. The combination of fingerprinting and chemical pattern recognition can comprehensively evaluate the quality of honeyed Eriobotryae Folium, and this method is stable and reliable, which can provide an effective reference basis for the habitat study of honeyed Eriobotryae Folium.

To improve the liquid chromatographic determination method of cefixime granules related substance.

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.

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.

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.

To explore the minimum effective inhibitory concentration of bacteriostatic agent in the prescription of human interferon α1b spray, and to determine the reasonable dosage of bacteriostatic agent.

Biological activity detection method was used to screen bacteriostatic agents in the prescription of human interferon α1b spray preparation, determine bacteriostatic agents. The bacteriostatic efficacy was determined according to the bacteriostatic efficacy test method of general principles 1121 of the Chinese Pharmacopoeia 2020 edition to determine the minimum effective bacteriostatic concentration of bacteriostatic agents. Staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans and Aspergillus niger were used as test strains to test the applicability of colony counting method. The dose screening test of bacteriostatic agent was designed to investigate the bacteriostatic effect of bacteriostatic agent with different concentrations on four kinds of experimental bacteria, and the reasonable dosage of bacteriostatic agent was selected.

Benzalkonium bromide was screened out as the bacteriostatic agent in the prescription of human interferon α1b spray. When the concentration of Benzalkonium bromide was 0.05-0.1 mg·mL^-1, its bacteriostatic efficacy against Staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans and Aspergillus niger met the grade A criteria.

The minimum effective bacteriostatic concentration of benzalkonium bromide in the prescription of human interferon α1b spray is determined to be 0.05 mg·mL^-1.

To compare the differences in identification tests of vacant gelatin capsules and enterosoluble vacant gelatin capsules in the four national pharmacopoeias, optimize the identification test methods and improve the specificity of identification results.

The biuret method was used to identify vacant gelatin capsules and enterosoluble vacant gelatin capsules, and an appropriate amount of adsorbed activated carbon was added to eliminate the masking effect of pigments in capsules.

The identification method was optimized, the pigment in the capsule solution was adsorbed by activated carbon, and the capsule solution showed a clarified colorless solution, which could produce a distinct violet after the color development by biuret reaction.

This method can significantly improve the specificity of vacant gelatin capsules and enterosoluble vacant gelatin capsules identification compared with domestic and foreign pharmacopoeia methods. It can provide scientific and reasonable revision suggestions for the optimization and improvement of the identification test of vacant gelatin capsules and enterosoluble vacant gelatin capsules in the Chinese Pharmacopoeia.