To classify the microbiological examination methods of live microecological products according to the results of suitability test for the enumeration method，and establish the decision-making method for microbiological examination of live microecological products.

The suitability test of the microbiological examination method of live microecological products was performed according to the requirements of the General Chapter 1105 in the Chinese Pharmacopoeia Vol Ⅳ. Escherichia coli，Staphylococcus aureus，Bacillus subtilis，Pseudomonas aeruginosa，Candida albicans and Aspergillus niger were used as the test strains. Tryptic Soy Agar，Sabouraud Dextrose Agar，Rose Bengal Agar and Rose Bengal Agar Ⅱ were used as medium.

For live microecological products composed of anaerobic bacteria or microorganisms with growth characteristics significantly different from the test strains，the suitability test for the method could be performed according to General Chapter 1105. For live microecological products containing Bacillus and enterococcus，the suitability test for the fungal enumeration method could be performed according to General Chapter 1105. Live microecological products could not be tested for suitability of the method due to the influence of the component microorganisms，gram-negative bacteria could be controlled using selective medium. In addition，some potentially harmful microorganisms could be controlled based on risk assessment according to the route of administration and the population of drug users.

This study provides a basis for the selection of the microbiological examination methods for live microecological products，and further complements and improves the quality standard system of live microecological products.

To establish a low-field and high-field nuclear magnetic resonance (NMR) technique for the determination of pyridoxine hydrochloride. To compare the differences between the results of method validation and sample content.

Using deuterated water as the solvent and maleic acid as the internal standard，method validation of quantitative nuclear magnetic resonance (qNMR) was accomplished with both 80 MHz low-field NMR and 500 MHz high-field NMR instruments. The content of pyridoxine hydrochloride was also determined.

The linearity of pyridoxine hydrochloride was good in the range of 10-30 mg·mL^-1，and the linear correlation coefficients were 0.999 8 and 0.999 6 for the low-field and high-field NMR，respectively. RSDs of the low-field and high-field NMR measurements were 1.4% and 0.040%，respectively. The contents were 100.4% and 100.8%，which were in agreement with the results from the mass balance method (100.0%). And the repeatability RSD was 0.20%. For the same concentration of the sample，the signal-to-noise ratio (S/N) of high-field NMR was about 100 times that of low-field NMR，and the half-peak width was 1/15 of that of low-field NMR.

Both low-field and high-field NMR instruments gave accurate results in the determination of pyridoxine hydrochloride content. However，low-field NMR was only suitable for compounds with simple structures. In the actual content determination，it is necessary to choose the appropriate instrument according to the structure and solubility of the sample to be tested.

To establish the quantitative analysis of multi-components by single marker（QAMS） method to simultaneously determine the contents of rutin，hyperoside，isoquercetin and quercetin in Zanthoxyli Pericarpium and Pericarpium Zanthoxyli Armati，and compare the differences in flavonoids contents.

Methanol extract of Zanthoxyli Pericarpium was analyzed on an Agilent Eclipse Plus C₁₈ (250 mm×4.6 mm，5 μm) chromatographic column. The mobile phase was acetonitrile(A)-0.1% formic acid(B) in a gradient elution. The flow rate was 1.0 mL·min^-1. The column temperature was 35 ℃，and the detection wavelength was 360 nm. The injection volume was 10 μL. Using hyperoside as the internal standard substance，the relative correction factors for the other 3 components were calculate and the flavonoids contents in Zanthoxyli Pericarpium and Pericarpium Zanthoxyli Armati were determined.

The 4 components had good linear relationship within their respective ranges (r≥0.999 9). The average recovery rates of Zanthoxyli Pericarpium were 99.3%-105.1% (n=6)，while thoes of Pericarpium Zanthoxyli Armati were 91.9%-99.8% (n=6). The relative average deviations of content of Zanthoxyli Pericarpium were 0.05%-3.37%，and the relative average deviations of content of Pericarpium Zanthoxyli Armati were 0.02%-3.28%. The results obtained by QAMS method were close to those obtained by the external standard method(ESM).

This method of QAMS method is accurate and reliable. The total amount of flavonoids in Pericarpium Zanthoxyli Armati is significantly higher than that in Zanthoxyli Pericarpium. Which provides reference for the comprehensive evaluation of the quality research of Zanthoxyli Pericarpium and Pericarpium Zanthoxyli Armati.

To establish an HPLC method for the simultaneous determination of eight components including salvianic acid A sodium，geniposidic acid，phellodendrine，salvianolic acid B，palmatine，berberine，atractylodin，tanshinone Ⅱ_A in Shuangshi Tonglin capsules.

The determination was performed on a Capcell Pak MG Ⅱ C₁₈ column (250 mm×4.6 mm，5 μm) with the mobile phase consisting of acetonitrile-water(containing 0.1% phosphoric acid)-water(containing 0.1% phosphoric acid and 0.2% triethylamine，pH 6.0) in a gradient mode at a flow rate of 1.0 mL·min^-1. The column temperature was set at 30 ℃，the injection volume was 10 μL，and the detection wavelength was 280 nm (0-13.4 min）for salvianic acid A sodium，238 nm (13.5-17.0 min) for geniposidic acid，280 nm （17.1-51.0 min）for phellodendrine，salvianolic acid B，345 nm（51.1.1-70.0 min）for palmatine，berberine，336 nm（70.1-78.0 min）for atractylodin and 268 nm(78.1-90.0 min)for tanshinone Ⅱ_A.

Salvianic acid A sodium，geniposidic acid，phellodendrine，salvianolic acid B，palmatine，berberine，atractylodin，tanshinoneⅡ_A had good linearities in their respective linear ranges with all linear correlation coefficients ≥ 0.999 5 and RSDs of the precision，repeatability and stability less than 2.0%. The average recoveries were 101.3%，98.2%，97.3%，98.1%，96.6%，97.9%，98.7%，99.6%，with RSDs lower than 2.0%. The contents of the above eight components in three batches of samples was 4.47-5.51 mg·g^-1，0.93-1.44 mg·g^-1，1.00-1.07 mg·g^-1，5.72-8.67 mg·g^-1，0.64-0.69 mg·g^-1，1.62-1.90 mg·g^-1，0.055-0.088 mg·g^-1，0.29-0.44 mg·g^-1，respectively.

The proposed method is rapid，sensitive and specific，which can be used for determination the contents of eitht components in Shuangshi Tonglin capsules.

To establish an HPLC method for the determination of related substances in olaparib raw materials.

By using YMC-Pack pro C₁₈ AS(150 mm×4.6 mm，3 μm) column，0.05 mol·L^-1 potassium dihydrogen phosphate (pH 3.0 adjusted with dilute phosphoric acid)-methanol-acetonitrile (90:5:5) was as mobile phase A and methanol-acetonitrile-water (45:45:10) was as mobile phase B，in gradient elution，with flow rate of 0.8 mL·min^-1. The column temperature was 30 ℃，the detection wavelength was 210 nm，and the injection volume was 10 μL.

The solvent blank did not interfere with the determination of relevant substances in the test solution，the known impurities Ⅰ-Ⅶ and unknown impurities in the system suitability solution were well separated in the chromatographic system. Olaparib had a good linear relationship with its peak area in the concentration range of 0.083-333.133 μg·mL^-1. The concentrations of impurities Ⅰ-Ⅶ were 0.05-3.0 μg·mL^-1，there were good linear relationships with their peak area，and their r were 0.999 7 or above. The average recoveries of impurities Ⅰ-Ⅶ were all above 92.0%，and RSDs were less than 4.0%.

The HPLC method for the detection of the related substances of olaparib raw materials has strong specificity，high sensitivity，high accuracy and good precision，which can meet the requirements for the detection of related substances of olaparib raw materials.

To develop a novel and efficient assay for the determination of free formaldehyde content in vaccines，and to compare the results with the method of the Chinese Pharmacopoeia(ChP) 2020 edition.

Vaccine samples were added directly into headspace vials without any pretreatment and tested after mixed with a new derivatization reagent，1% p-toluenesulfonic acid-ethanol solution (1% TsOH-EtOH solution). The concentration of the reagent，the dosage and the optimal derivatization conditions (headspace incubation temperature and time) were tested and confirmed. A DB-624 gas capillary column was used with temperature programming. The detector was a hydrogen-ion flame detector (FID) and the sample was injected in headspace.

The linear range was 0.25-100 μg·mL^-1（r=0.999 5），the detection limit and the quantification limit were 0.10 μg·mL^-1 and 0.25 μg·mL^-1，respectively. The recovery rates of several kinds of vaccines were all over 94%，and the RSDs were all less than 6%，which were in line with the requirements of specificity，precision and durability. There were no significant differences between the results of multiple batches and those determined by ChP 2020 methods.

In this paper，a novel derivatization reagent (1% TsOH-EtOH solution) was developed and validated for the determination of free formaldehyde content in vaccines，which is simple，efficient and can achieve high-throughput detection. The method can just solve the problems in other current detection methods. The method of derivatization headspace gas chromatography for the determination of free formaldehyde content is applicable to vaccines and other biologics，and provide a reference for chemicals，traditional Chinese medicine and excipients.

To establish an UPLC quantitative analysis method for the simultaneous determination of 13 components in Yankening tablets, including phellodendrine, coptisine, baicalin, palmatine, berberine, wogonoside, baicalein, aloe-emodin, rhein, wogonin, emodin, chrysophanol, physcion.

Agilent Eclipse Plus C₁₈(100 mm×2.1 mm, 1.8 μm) column was used with acetonitrile -0.1% phosphoric acid as mobile phase, and gradient elution at a flow rate of 0.3 mL·min^-1. The detection wavelengths were 210 nm and 254 nm. The column temperature was 40 ℃.

Phellodendrine hydrochloride, coptisine hydrochloride, palmatine hydrochloride, berberine hydrochloride, baicalin, wogonoside, baicalein, aloe-emodin, rhein, wogonin, emodin, chrysophanol, physcion showed good linear relationships within their concentration range of 0.97-48.63 μg·mL^-1, 0.95-47.52 μg·mL^-1, 0.86-43.15 μg·mL^-1, 0.86-43.19 μg·mL^-1, 0.89-44.37 μg·mL^-1, 1.00-49.84 μg·mL^-1, 1.02-51.01 μg·mL^-1, 0.97-48.31 μg·mL^-1, 0.99-49.50 μg·mL^-1, 1.04-51.80 μg·mL^-1, 1.00-50.04 μg·mL^-1, 1.00-49.80 μg·mL^-1, 1.01-50.64 μg·mL^-1. The average recoveries(n=6) were 95.2%, 96.7%, 95.9%, 98.3%, 94.1%，97.6%, 99.2%, 96.6%, 95.5%, 97.2%, 97.0%, 97.8%, 98.7%, RSD values were all less than 2.0%. The contents of the 13 chemical components in 3 batches of samples were 1.367-1.488 mg·g^-1(calculated as phellodendrine hydrochloride), 0.378-0.412 mg·g^-1(calculated as coptisine hydrochloride), 4.611-5.505 mg·g^-1, 0.324-0.407 mg·g^-1(calculated as palmatine hydrochloride), 3.665-3.878 mg·g^-1(calculated as berberine hydrochloride), 1.107-1.682 mg·g^-1, 0.392-0.941 mg·g^-1, 0.076-0.105 mg·g^-1, 0.097-0.116 mg·g^-1, 1.059-1.213 mg·g^-1, 0.149-0.167 mg·g^-1, 0.213-0.239 mg·g^-1, 0.047-0.059 mg·g^-1.

The method is accurate, high analysis efficiency, good repeatability, it can be used to control the quality of Yankening tablets.

To establish the UPLC-MS/MS method for simultaneous determination of 9 components (nicotinic acid, kaempferol, swertisin, quercetin, luteolin, rutin, vitexin, spinosin, salicylic acid) in Desmodium caudatum (Thunb.) DC. and construct a back propagation(BP) neural network model to predict the origin of Desmodium caudatum (Thunb.) DC. from different habitats.

The chromatographic separation was achieved on an Agilent Zorbax SB C₁₈ column (50 mm×3.0 mm，1.8 μm). The mobile phase consisted of methanol -0.1% acctic acid (containing 0.02 mol·L^-1 ammonium acetate) at a flow rate of 0.3 mL·min^-1 with gradient elution, the MS analysis were performed by multiple reaction monitoring (MRM) under ESI⁺ and ESI. A correlation analysis was conducted on the contents of each component, and a BP neural network model was constructed to distinguish Desmodium caudatum (Thunb.) DC. from different habitats.

Under the optimized conditions, 9 components(nicotinic acid, kaempferol, swertisin, quercetin, luteolin, rutin, vitexin, spinosin, salicylic acid) showed good linear relationships in the ranges of 0.388 8-38.88 ng·mL^-1, 10.07-1 006.6 ng·mL^-1, 34.22-34 221.6 ng·mL^-1, 3.944-394.4 ng·mL^-1, 2.124-212.4 ng·mL^-1, 4.344-434.4 ng·mL^-1, 46.50-4 650.1 ng·mL^-1, 1.649-164.9 ng·mL^-1, 4.880-488.0 ng·mL^-1, respectively (r>0.995 1), whose average recoveries were 96.9%-103.9% (RSDs<1.9%). The contents of the above nine components in 40 batches of Desmodium caudatum (Thunb.) DC. were 1.657-7.407 μg·g^-1, 15.801-64.488 μg·g^-1, 1 068.348-4 270.780 μg·g^-1, 10.608-123.228 μg·g^-1, 3.897-16.802 μg·g^-1, 1.269-97.834 μg·g^-1, 405.285-1 955.796 μg·g^-1, 13.614-36.124 μg·g^-1, 4.417-87.509 μg·g^-1, respectively. According to correlation analysis, four components (swertisin, rutin, spinosin, and luteolin) in Desmodium caudatum (Thunb.) DC. showed a highly linear positive correlation, indicating that these four components had a certain synergistic effect in Desmodium caudatum (Thunb.) DC.. The BP neural network model was constructed to predict Desmodium caudatum (Thunb.) DC. from different habitats, and the accuracy of the test set reached 92.3%.

The method is simple, sensitive and efficient, and can be used for the rapid determination of the components in Desmodium caudatum (Thunb.) DC.. Using the BP neural network model to predict the habitats plays a significant role in tracing the origin of Desmodium caudatum (Thunb.) DC..

To establish the RP-UPLC-PDA method for simultaneous determination of triptolide，triptonide, triptophenolide, wilforine, wilforlide A and celastrol in Tripterygii Radix.

Tripterygii Radix were extracted with ethyl acetate and the extracts were dissolved and separated by methanol. The six components were determined by RP-UPLC-PDA method. The chromatographic column was Acquity^TM UPLC BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm), the column temperature was 30 ℃, the injection volumn was 2 μL, the flow rate was 0.4 mL·min^-1 and the mobile phase was acetonitrile (A)-0.1% formic acid (B).

The linear relationship of six components was good (0.999 2≤r≤0.999 7) in the concentration ranges. The average recoveries were 99.2%-103.1% and RSDs were 1.2%-2.9%. The contents in 10 batches of Tripterygii Radix from different habitat were determined. The results showed that the contents of Tripterygii Radix in prepared pieces from different producing areas were different. The highest content of triptolide was 140.2 μg·g^-1, and the lowest content was 103.2 μg·g^-1. The highest content of triptonide was 224.7 μg·g^-1 and the lowest content was 112.2 μg·g^-1. The highest content of triptophenolide was 306.7 μg·g^-1 and the lowest content was 189.6 μg·g^-1. The highest and lowest contents of wilforine were 283.2 μg·g^-1 and 211.2 μg·g^-1. The highest content of wilfhabitat was 31.2 μg·g^-1 and the lowest content was 16.8 μg·g^-1. The highest content of celastrol was 87.6 μg·g^-1, and the lowest content was 52.1 μg·g^-1.

The RP-UPLC-PDA method can simultaneously determine six components in Tripterygii Radix. The method is reliable and stable, which is suitable for quantitative analysis and determination of Tripterygii Radix.