Construction of universal quantitative models for the determination of cefoperazone sodium/sulbactam sodium for injection from different manufacturers using near-infrared reflectance spectroscopy

To develop near-infrared （NIR） reflectance spectroscopic methods for the quantitative analysis of cefoperazone sodium/ sulbactam sodium from different manufacturers for injection powder medicaments. Various powders of cefoperazone sodium/ sulbactam sodium were directly analyzed by non-destructive NIR reflectance spectroscopy using the spectrometer EQUINOX55. Two quantitative methods via integrating sphere （IS） and fiberoptic probe （FOP） models were explored from 6 batches of commercial samples and 42 batches of laboratory samples at a content ranging from 30% to 70% for cefoperazone and 60% to 20% for sulbactam. The root mean square errors of cross validation （RMSECV） and the root mean square errors of prediction （RMSEP） of IS were 1.79% and 2.85%, respectively, for cefoperazone sodium, and were 1.86% and 3.08%, respectively, for sulbactam sodium; and those of FOP were 2.93% and 2.92%, respectively, for cefoperazone sodium, and were 2.23% and 3.01%, respectively, for sulbactam sodium. Based on the ICH guidelines and Ref. 12, the quantitative models were then evaluated in terms of specificity, linearity, accuracy, precision, robustness and model transferability. The non-destructive quantitative NIR methods used in this study are applicable for rapid analysis of injectable powdered drugs from different manufacturers.

A Novel Sample Introduction Technique for the Simultaneous Determination of As,Se,Ge and Hg in Chinese Medicinal Material

A novel technique of Moveable Reduction Bed Hydride Generator（MRBHG）was applied tohe hydride generation or cold vapor generation of As，Se，Ge，and Hg existing In TraditionalChinese Medicinal Material（TCM）．The simultaneous determination of the multi－elements wasperformed with ICP－MS．A solid reduction system involving the use of potassiumtetraborohydride and tartaric acid was applied to generating metal hydride or cold vaporefficiently．The factors affecting the metal cold vapor generation were studied．The mainadvantage of the technique is that only a 4μL volume of sample was required for the cold vapor

RAPD Technique Used to Determine the Purity of Hybrid Hot Pepper Seeds

Two hybrid hot pepper varieties Xiangyan 5 and Xiangyan 10, and their parents were analyzed the polymerase chain reaction with MJ /PT 200 Peltrier Themal Cycler and DS 800 White-ultravilot Transilluminator to set up a RAPD system adaptable to the purity determination of the hy-brid seeds. Among the 39 random primers, 2 and 4 primers were found to be used effectively in Xiangyan 5 and Xiangyan 10 respectively.

Determination of Trace Impurities of Rare Earth Elements in High Purity Yttrium Oxide by ICPMS

Determination of trace rare earth elements(REEs)in 99. 999% purity yttrium oxide using the inductively coupled plasma mass spectrometric technique (ICPMS) has been developed. Instrumental parameters and factors affecitng analytical results have been studied and then optimized.Samples are analyzed directly following an acid digestion without separation or preconcentration and with limit of detection of 0. 003～0. 02 ng/ml, precision of ±5. 4%(cofficient of variation)and recovery of 90～115%. Correction for isobaric interferences from oxide ions and hydroxide ions is made mathematically. Special internal standard procedures are used to compensate drift in metal:metal oxide ratios and sensitivity. The analytical results of several samples are accurate as compared with inductively coupled plasma atomic emission spectrometry (ICPAES) and spark source mass spectrometry (SSMS).

Establishment and evaluation of O/W type-based microemulsion on crossbow medicine of the Miao ethnic group

Background:Crossbow medicine needle is a traditional external therapy.However,acupuncture pain,inaccurate administration,secondary infection,and poor patient compliance limit the application of specialty therapies.Since the most effective components of crossbow medicine are lipid-soluble,the crossbow medicine needle was prepared as an innovative O/W-type microemulsion to solve these problems.In this study,the crossbow medicine microemulsion preparation method was established and its quality was evaluated.Methods:A single factor and pseudoternary phase diagram,combined with a D-optimal mixture design,optimized the formulation of crossbow medicine microemulsion through particle size,polydispersity index,zeta potential,microstructure,and contents of benzoyl neoaconitine,benzoyl hypoaconitine,neoaconitine,periplocin,and methyl salicylate to evaluate the final prescription.Results:The best prescription for preparing crossbow medicine microemulsion is 0.1500 g crossbow medicine dry extract,0.1500 g isopropyl myristate,0.8625 g polyoxyethylene castor oil-35,0.2875 g ethanol,3.700 g water,and 5.1500 g microemulsion.The prepared microemulsion is an oil-in-water type with a clear and transparent appearance.Its average particle size is 19.83±0.78 nm,average polydispersity index is 0.15±0.02,and average zeta potential is−0.51±0.1 mV.The pH value is 5.17±0.02.The microstructure of crossbow medicine microemulsion illustrated a uniform distribution of spherical oil globules.The average contents of benzoyl neoaconitine,benzoyl hypoaconitine,neoaconitine,periplocin,and methyl salicylate were 13.34,113.05,43.45,628.27 and 27.93μg/g,respectively.Conclusion:The preparation process of crossbow medicine microemulsion is reasonable and feasible.The method to determine the content is accurate and straightforward,laying the foundation for further research.

A Preliminary Study on the Quality Standard of Raphanus sativus L. Produced in Guizhou Province

[Objectives]This study was conducted to analyze the Raphanus sativus L.medicinal materials from different origins and batches in Guizhou Province to explore its quality standards.[Methods]The plant morphology,material shape and microscopic characteristics of R.sativus were identified;and qualitative identification was performed by the TLC method.[Results]The plant morphology,material shape and microscopic characteristics of the R.sativus medicinal materials were described;and the TLC identification method of the R.sativus medicinal materials was established,with clear spots,good separation,and good specificity.[Conclusions]The method is accurate,simple,highly sensitive,interference-free,has good reproducibility,and can be used as a data support for the formulation of quality standards for R.sativus medicinal materials.

Determination of vanadium in food and traditional Chinese medicine by graphite furnace atomic absorption spectroscopy

Various experimental conditions were described for the vanadium determinationby graphite furnace atomic absorption spectroscopy (GFAAS). The experiments showed that whenatomization took place under the conditions where the combination of a pyrolytic coating graphitetube and fast raising temperature were used and the temperature was stable, the signal peak shapescould be improved, the sensitivity was enhanced, and the memory effect was removed. The vanadium infood and traditional Chinese medicinal herbs can be accurately determined using the standard curvemethod.

Purity and Uncertainty Study of CRM Betulin by DSC

Betulin(BE)can be obtained from many plants,such as those belonging Betulaceae family,and pharmacological investigations showed its notable biological properties and good potential for food and pharmaceutical development.We investigated the homogeneity,stability,purity,and uncertainty of a newly certified reference material(CRM)of BE.The certified purity value for the CRM of BE was 99.56%with an extended uncertainty of 0.07%(k=2,P=0.95),as determined by differential scanning calorimetry(DSC).In this study,DSC was used for the first time for purity determination of BE.Given its high accuracy,precision,and reproducibility,DSC can be used as an alternative technique for purity determination of CRMs in the pharmaceutical and food industry.

Study on Quantity Value Transfer Relationship of Triplostegia glandulifera Wall.ex DC. Decoction Pieces-Standard Decoction-Finished Product

[Objectives] In order to develop Triplostegia glandulifera Wall.ex DC. into foromula granules, a high performance liquid chromatography (HPLC) determination method and a TLC identification method for loganic acid in decoction pieces, standard decoction and formula granules of T. glandulifera were established, and the quantity value transfer relationship of T. glandulifera pieces-standard decoction-formula granules was investigated.[Methods] An Agilent 1260 II high performance liquid chromatograph and a Waters Symmetry C 18 column (4.6 mm×250 mm, 5 μm) were used to perform gradient elution with acetonitrile-0.1%phosphoric acid solution as the mobile phase at a column temperature of 30 ℃ and a flow rate of 1 mL/min, and the detection wavelength was 240 nm. The TLC identification method of T. glandulifera was established using ethyl acetate-methanol-water (10 : 2 : 1) as the developer, and examination was carried out under a UV lamp (254 nm). The quantity value transfer law was analyzed by using the extract yield, the content of loganic acid and TLC chromatograms as the main evaluation indexes.[Results] The method for the determination and identification of loganic acid is stable, reproducible and reliable. The average yield, average loganic acid content and average loganic acid content transfer rate of 3 batches of T. glandulifera formula granules were, respectively, 18.7%, 41.1 mg/g and 43.1%, each of which was within corresponding range of mean±3SD of the 15 batches of standard decoction.[Conclusions] The content determination and TLC identification methods of loganic acid can be used to evaluate the quality of T. glandulifera formula granules. This study provides data basis for further research on T. glandulifera formula granules, and promotes the modernization of medicines for ethnic minorities.

Development and Validation of an HPLC Method for Simultaneous Determination of Nine Active Components in ‘Da-Chai-Hu-Tang’

In this study, a simple, reliable and accurate method for the simultaneous separation and determination of naringin, hesperidin, neohesperidin, baicalin, wogonoside, baicalein, wogonin, emodin and chrysophanol in ‘Da-Chai-Hu-Tang’ was developed by reverse-phase high-performance liquid chromatography (RP-HPLC). The chromatographic separation was performed on an Agilent ZORBAX C18 column (250 mm × 4.6 mm i.d., 5.0 μm), and the mobile phase composed of methanol and water containing 1% (v/v) acetic acid was used to elute the targets in a gradient elution mode. The flow rate and detection wavelength were set at 0.8 ml/min and 280 nm, respectively. All calibration curves of the nine components expressed good linearities (r2≥0.9992) within the tested ranges. The RSD values demonstrated the intra- and inter-day precisions were less than 2.89%, and the recoveries of the investigated compounds were between 96.22% and 105.28%. The proposed method is simple, precise, specific, sensitive, and successfully applied to determine the nine marker compounds in ‘Da-Chai-Hu-Tang’ for quality control.

DETERMINATION OF OSMOTIC VELOCITY OF LIQUID MEDICINE IN POROUS CERAMIC TUBE

Acquiring detail knowledge of the situation about release of medicial liquid is a key problem in clinical practice. By means of imitating the condition in the human body, the authors determined the osmotic velocity of anticarcinogen, antituberculotic, antibiotic and other medicines in porous ceramic tubes. In this paper, the methods to determine the osmotic velocity of anticarcinogen and to calculate the experimental data are mainly introduced.

Quality Evaluation of Yi Medicine "Qibujing" Based on Determination of Water Content and Ash Content

[Objectives]To determine the water content,total ash content and acid-insoluble ash content of Yi medicinal material"Qibujing",so as to provide experimental basis for establishing the Quality Standard(Draft)of Yi Medicinal Material"Qibujing"in Sichuan Province.[Methods]According to the second method(drying method)in 0832 water content determination method and 2301 ash content determination method in Chinese Pharmacopoeia(2015 Edition),it was determined,respectively,and the data were processed by IBM SPSS Statistics 26 and DPS 7.05 data processing system.[Results]All the 14 batches of sample met the stipulation that the water content should not exceed 12.0%,the total ash content should not exceed 8.0%,and the acid-insoluble ash content should not exceed 1.5%under"Guan Zhong-(Qibujing)"in the 2005 edition of Yunnan Traditional Chinese Medicine Standard.There was a negative correlation between water content,acid-insoluble ash content and altitude,and a positive correlation between total ash content and altitude.[Conclusions]It is suggested that Quality Standard(Draft)of Yi Medicinal Material"Qibujing"in Sichuan Province stipulate that the water content should not exceed 12.0%,the total ash content should not exceed 8.0%,and the acid-insoluble ash content should not exceed 1.5%.

GC-TOF-MS技术快速鉴定抗风湿痛胶囊中添加的西药成分

应用高分辨GC-TOF-MS对抗风湿痛胶囊中的未知西药成分进行快速鉴定。使用不同极性的有机溶剂进行提取,将提取物分别离心,取上清液进行气质联用分析,并借助Nist2002数据库进行鉴定,用精确分子质量和元素分析进行确证。分析发现,此抗风湿痛胶囊中添加了甲氧苄氨嘧啶、磺胺甲恶唑、安定、可待因、茶碱等5种西药。用液质联用仪对甲氧苄氨嘧啶、磺胺甲恶唑进行了定量分析。该方法可用于未知混合物的分析,同样适用于中药制剂中其他西药成分的快速检出。

Study on Quality Standard of Zhuang Medicine Buddlejae Flos

[Objectives]This study was conducted to explore the quality control method and establish the quality standard of Zhuang medicine Buddlejae Flos.[Methods]The microscopic identification method was adopted to identify the characters and microscopic characteristics of dried Buddlejae Flos in combination with traditional experience.The moisture,ash,acid-insoluble components and extracts of Buddlejae Flos were determined with reference to general rules of Chinese Pharmacopoeia(2015 edition).TLC identification was performed.Liquid chromatography-mass spectrometry(LC-MS)was used to determine the contents of linarin and verbascoside in Buddlejae Flos,and gas chromatography-mass spectrometry(GC-MS)was adopted to detect pesticide residues in Buddlejae Flos.Heavy metal elements As,Cd and Pb were detected by inductively coupled plasma mass spectrometry(ICP-MS).[Results]The established method is simple and accurate.Clear spots were observed on the thin layer chromatograms,and the resolution was good.The average value of moisture content was 12.24%;the average value of ash content was 5.1%;the average value of acid-insoluble content was 7.5%;and the average value of extract content was 27.3%.The regression equation of rutin in Buddlejae Flos was y=11.896x-0.0049,R^(2)=0.9996,and the contents of linarin and verbascoside were 5680 and 2080 mg/kg,respectively.No pesticide residues and heavy metals were detected in the medicinal materials of Buddlejae Flos.[Conclusions]This study can provide reference for the quality standard control of Guangxi Zhuang medicine Buddlejae Flos.

Research of Quality Standards for Stachydrine Hydrochloride in Chinese Medicine TJF Granule

A high-performance liquid chromatographic method was applied to the determination of stachydrine hydrochloride concentration in TJF granule (Chinese name: Tiao-Jing-Fang), using a mobile phase of methanol-acetonitrile (50:50, v/v) by the Agilent Kromasi NH2 column (250 mm × 4.6 mm, 5 μm, S/N: 22N25110). Detection wavelength was 201 nm. The result revealed good linearity of stachydrine hydrochloride and was obtained within the range of 0.20 - 1.98 μg/mL (R = 0.9995). The average recovery was 97.01%;the relative standard deviation (RSD) was 0.19%. To the best of our knowledge, this is the first report dedicated to the determination of stachydrine hydrochloride by the evaporative light scattering detector-high-performance liquid chromatographic (ELSD-HPLC) method.

Extraction Process of Zhuang Medicine Fumigation Lotion

[Objectives]To establish the extraction process and quality standard method of Zhuang medicine fumigation lotion.[Methods]The orthogonal design method was employed to optimize the water extraction process with the amount of water added,decocting time and extraction times as factors,and syringin content and dry extract yield as indexes.The content of syringin was determined by high performance liquid chromatography.[Results]The best water extraction process was:soaking in water for 1 h,decocting twice,added 10 times the amount of water each time,decocting for 1 h.The average content of syringin in 3 batches was 0.98 mg/g,and the average dry extract yield was 26.07%.[Conclusions]The project adopts water extraction method to prepare Zhuang medicine fumigation lotion,which has the characteristics of high efficiency and suitable for large-scale production.The quality control method is reliable,rapid and accurate,and can effectively control the quality of the lotion.

Research progress on fluorescence analysis of antitumor Chinese medicine components

This paper classifies the anti-tumor traditional Chinese medicine's fluorescence analysis and finds that its research content mainly includes two aspects:the application of fluorescence analysis in the determination of the effective component content of anti-tumor traditional Chinese medicine;the study of the combined use of fluorescence imaging technology and the drug.According to literature analysis,it is found that although the research on the fluorescence analysis of anti-tumor Chinese medicine components is in a good state of development,it still needs to explore further in the identification of unknown components and deeper research on known components.Therefore,it can provide a certain basis for clinical guidance of tumor patients.

NOVEL APPROACHES FOR THE DETERMINATION OF MULTIPLE PARTICULAR PESTICIDES IN TRADITIONAL CHINESE MEDICINES WITH COMPLEX MATRICES

The pesticide contamination of Traditional Chinese Medicines(TCMs)takes different ways,which caused the complexity of pesticide residues.The effective control of pesticide residues and the establishment of relevant detection methods are very important for ensuring the safety of TCMs.Our group has been committed to the determination of pesticide residues in TCMs for years.

A SERIES OF STRATEGIES FOR SOLVING THE SHORTAGE OF REFERENCE STANDARDS FOR MULTI-COMPONENTS DETERMINATION OF TRADITIONAL CHINESE MEDICINE

The shortage of reference standards has become the bottleneck of quality control of TCMs.In this study,a series of strategies,including one single reference standard to determine multi-compounds(SSDMC),quantitative analysis by standardized reference extract(QASRE),and quantitative nuclear magnetic resonance

CURRENT AND FUTURE APPROACHES TO THE QUALITY OF CONTROL OF CHINESE HERBAL MEDICINES

Quality of control of Chinese herbal medicines is currently mainly based on specifications of pharmacopoeias.Challenges are the limited specificiity of some of these methods,the use of various grades and processed materials,which cannot easily be distinguished,and the increasing use of granules,which are so far not considered in most pharmacopoeias.For identity and purity testing,microscopy and TLC fingerprint analysis are