Improvement of the quality standard of Gerbera piloselloides / 中国药房

OBJECTIVE To improve th e quality standard for Gerbera piloselloides. METHODS The properties of G. piloselloides were observed and microscopic identification was conducted for powder. The moisture ，total ash ，acid-insoluble ash and ethanol-soluble extract were detected according to the method stated in 2020 edition of Chinese Pharmacopoeia （part Ⅳ）. The contents of nodakenin，luteolin-7-O-β-D-lutinoside，luteoloside，apigenin-7-O-β-D-lutinoside，apigenin-7-O-β-D-glucopyranoside and marmesin were determined by high performance liquid chromatography method. RESULTS G. piloselloides were shrunken ，densely covered with thick white cotton wool ，with many fibrous roots ；the surface was taupe or gray-brown ；its texture was brittle and easy to break ；the cross section was yellow-white ，and there was an obvious small wooden heart in the center. Its powder was tan ， and non-glandular hairs ，stone cells ，calcium oxalate cubes ，ducts，fibers could be seen unde r microscope. The measured values of moisture，total ash ，acid-insoluble ash and alcohol-soluble extract ， for 15 batches of samples were 8.63％-11.34％，10.39％-14.93％， 3.29％-6.37％ and 9.03％-15.02％，respectively；average values were 10.01％，12.26％，4.61％，12.36％. The linear ranges of nodakenin，luteolin-7-O-β-D-rutinoside，luteoloside，apigenin- 7-O-β-D-lutinoside，apigenin-7-O-β-D-glucopyranoside and marmesin we re 3.87-154.88，1.64-65.41，1.60-64.00，1.92-76.96， 1.27-50.93，0.40-15.89 μg/mL，respectively（r≥0.999 1）. RSDs of precision ，stability（24 h）and repeatability tests were all less than 3％. The average recoveries were 101.88％，100.89％，102.64％，95.75％，96.71％ and 103.48％，respectively；RSDs were 0.55％，0.43％，0.34％，0.49％，0.47％ and 0.37％，respectively（n＝6）；the contents of above 6 components were 0.152 7-0.852 2， 0.084 5-0.669 7，0.136 7-0.961 0，0.126 0-1.193 2，0.128 8-1.102 2，0.046 9-0.678 0 mg/g. CONCLUSIONS The established method can be used for the quality control of G. piloselloides . It is preliminarily proposed that the moisture in G. piloselloides is not more than 12.0％；the total ash is not more than 15.0％，the acid-insoluble ash is not more than 6.0％，the alcohol-soluble extract is not less than 9.0％；the contents of luteoloside and apigenin- 7-O-β-D-glucopyranoside are not less than 0.016％.

Application of HPLC-DAD for the quantification of Lycorine in Galanthus elwesii Hook

ABSTRACT In the present study, a reversed-phase high-performance liquid chromatographic method has been used for the quantitative determination of lycorine in the aerial parts and bulbs of G. elwesii Hook. A simple method for the extraction of lycorine in low mass plant samples was employed utilizing pre-packed columns with diatomaceous earth (Extrelut(r)). The chromatographic separation was performed using an isocratic system with a mobile phase of trifluoroacetic acid-water-acetonitrile (0.01:92.5:7.5, v/v/v) applied at a flow rate 1 mL min-1 using diode array detector. The content of lycorine in the bulbs and aerial parts of G. elwesii collected from Demirci (Manisa) was found as 0.130 and 0.162 %, respectively. Additionally, in the bulbs of the specimens collected from Sogucak (Balikesir), lycorine was quantified as 0.055 %, whereas in the aerial parts, it was determined as 0.006 %. The method was validated partially with respect to system specificity, linearity, accuracy, precision, limits of detection (LOD) and quantitation (LOQ). Validation procedures displayed that the method was specific, accurate and precise.

A simple HPLC method for the determination of halcinonide in lipid nanoparticles: development, validation, encapsulation efficiency, and in vitro drug permeation

ABSTRACT Halcinonide is a high-potency topical glucocorticoid used for skin inflammation treatments that presents toxic systemic effects. A simple and quick analytical method to quantify the amount of halcinonide encapsulated into lipid nanoparticles, such as polymeric lipid-core nanoparticles and solid lipid nanoparticles, was developed and validated regarding the drug's encapsulation efficiency and in vitro permeation. The development and validation of the analytical method were carried out using the high performance liquid chromatography with the UV detection at 239 nm. The validation parameters were specificity, linearity, precision and accuracy, limits of detection and quantitation, and robustness. The method presented an isocratic flow rate of 1.0 mL.min-1, a mobile phase methanol:water (85:15 v/v), and a retention time of 4.21 min. The method was validated according to international and national regulations. The halcinonide encapsulation efficiency in nanoparticles was greater than 99% and the in vitro drug permeation study showed that less than 9% of the drug permeated through the membrane, indicating a nanoparticle reservoir effect, which can reduce the halcinonide's toxic systemic effects. These studies demonstrated the applicability of the developed and validated analytical method to quantify halcinonide in lipid nanoparticles.

Development and validation of a stability indicating HPLC method to determine diltiazem hydrochloride in tablets and compounded capsules

ABSTRACT A stability indicating HPLC method to determine diltiazem hydrochloride (DTZ) in tablets and compounded capsules was developed and validated according to Brazilian and the International Conference on Harmonization (ICH) guidelines. The separation was carried out on a Purospher Star® C18 (150 x 4.6 mm i.d., 5 µm particle size, Merck Millipore) analytical column. The mobile phase consisted of a 0.05% (v/v) trifluoroacetic acid aqueous solution and a 0.05% trifluoroacetic acid methanolic solution (44:56, v/v). The flow rate was 1.0 mL.min-1 with a run time of 14 minutes. The detection of DTZ and degradation products (DP) was performed at 240 nm, using a diode array detector. The method proved to be linear, precise, accurate, selective, and robust, and was adequate for stability studies and routine quality control analyses of DTZ in tablets and compounded capsules.

HPLC method development and validation for the estimation of Axitinib in rabbit plasma

ABSTRACT A rapid, sensitive, and accurate high performance liquid chromatography for the determination of Axitinib (AN) in rabbit plasma is developed using crizotinibe as an internal standard (IS). Axitinib is a tyrosine kinase inhibitor, used in the treatment of advanced kidney cancer, which works by slowing or stopping the growth of cancer cells. The chromatographic separation was performed on a Waters 2695, Kromosil (150 mm × 4.6 mm, 5 µm) column using a mobile phase containing buffer (pH 4.6) and acetonitrile in the ratio of 65:35 v/v with a flow rate of1 mL/min. The analyte and internal standard were extracted using liquid-liquid extraction with acetonitrile. The elution was detected by photo diode array detector at 320 nm.The total chromatographic runtime is 10.0 min with a retention time for Axitinib and IS of 5.685, and 3.606 min, respectively. The method was validated over a dynamic linear range of 0.002-0.2µg/mL for Axitinib with a correlation coefficient of r2 0.999.

SEDATION AND HYPNOSIS EFFECT OF JIAOTAI PILLS ON RAT INSOMNIA IN PCPA RAT MODEL / 现代医院

Objective To discuss the sedative and hypnotic effect of Jiaotai Pills on insomnia in PCPA rat model .Methods The PCPA ( PCPA acid) rats insomnia model was established, and the rats were divided into the model group, high, middle and low dosage of Jiaotai Pills group, and diazepam positive control group.The high performance liquid detective method was adopted to observe the effect of Jiaotai Pills on rat insomnia and hypothalamus neurotransmitters 5-HT and GABA.Results Compared with the model group, there existed significant difference in the insomnia state of rats and the central neurotransmitters 5 -HT in the high and middle dosages of Jiaotai Pill group and diazepam group.However, in the comparison of the high and middle dosages of Jiaotai Pill group and the model group, there was no significant difference in GABA in the central nervous system .Conclusion Jiaotai Pills has sedative and hypnotic efficacy.Its mechanism may be related to the effects of central neurotransmitter 5 -HT.Its relationship with GABA in the central nervous system is not obvious.The research has significant influence on the further development of Jiaotai Pills.