OBJECTIVE To explore whether pyridoxine can protect acute kidney injury caused by cisplatin and to analyze its specific mechanism. METHODS After establishing an in vitro model of cisplatin-induced damage in HK-2 cells, different concentrations of pyridoxine were administered and cell survival was detected using SRB, the expression of apoptosis-related and antioxidant proteins were detected by Western blotting, and the activity of reactive oxygen species(ROS) and superoxide dismutase(SOD) were detected by kits. A cisplatin-induced mouse kidney injury model was further established, and the serum urea nitrogen level was detected after the administration of 40 mg·kg–1 pyridoxine treatment, the results of hematoxylin-eosin staining in renal tissue were analyzed, and the expression of NRF2 was detected by Western blotting. RESULTS Pyridoxine could protect kidney injury caused by cisplatin in HK-2 cells and mouse in vivo. In HK-2 cells, pyridoxine down-regulated ROS level, up-regulated SOD enzyme activity, and up-regulated the expression of NRF2 and its downstream antioxidant-related gene HO-1. Pyridoxine significantly reduced the level of serum urea nitrogen, repaired kidney tissue damage, and up-regulated the expression of NRF2 in kidney injury mice. CONCLUSION Pyridoxine protects against cisplatin-induced kidney injury through enhancing the level of anti-oxidative stress.

OBJECTIVE To evaluate the effects of different fresh processing methods on the quality of Puerarial Lobatae Radix using entropy weight TOPSIS model and multi-index. METHODS By optimizing the specifications of fresh cut(thick slices of 2, 3, 4 mm thick, the side length of 0.5, 1, 1.5 cm), drying method(drying at 45, 65, 85 ℃, freeze drying) and other parameters, Puerarial Lobatae Radix medicinal materials were processed at the origin, and Puerarial Lobatae Radix decoction pieces were obtained. Using the content of 3′-hydroxy puerarin, puerarin, puerarin apioside, 3′-methoxy puerarin, puerarin-6″-O-xyliside, daidzin, genistin, daidzein, ethanol soluble extractives, as well as moisture and ash content limits as evaluation indicators, through the entropy and TOPSIS method to analyze the index component data and optimizing the Puerarial Lobatae Radix best when fresh herbs processing technology. RESULTS Different fresh processing methods had a certain influence on the content of the index components of Puerarial Lobatae Radix, and the best cutting specification was 0.5 cm thick, and the best drying method was freezed drying. CONCLUSION The entropy weight TOPSIS method can be used to evaluate the effects of different processing methods on the quality of Puerarial Lobatae Radix, and the best processing technology obtained has good stability and repeatability, which can provide guidance for the standardization of processing technology of Puerarial Lobatae Radix.

OBJECTIVE To study the best extraction process of β-asarone from Acori Tatarinowii Rhizoma by ethanol heating reflux method, and to explore the antioxidant activity of different segments. METHODS With β-asarone from Acori Tatarinowii Rhizoma as the evaluation index to optimize the extraction method. On the basis of a single factor experiment, the effects of ethanol concentration, solid-liquid ratio and extraction time on the extraction amount of β-asarone from Acori Tatarinowii Rhizoma were investigated by orthogonal design and response surface methodology. After the optimal extraction process was determined, the antioxidant activities of different segments were studied. RESULTS The optimum extraction process of β-asarone from Acori Tatarinowii Rhizoma was as follows: ethanol concentration was 95%, solid-liquid ratio was 1∶20 g·mL–1 and extraction time was 2.5 h. Under these conditions, the extraction amount of β-asarone from Acori Tatarinowii Rhizoma was 0.918 7 mg·g–1. The results of in vitro antioxidant activity showed that the order of antioxidant capacity was ethyl acetate>petroleum ether>ethanol>n-butanol. Among them, the ethyl acetate fraction had the strongest antioxidant activity, with good ability to scavenge DPPH and ABTS free radicals, and had certain reduction ability. CONCLUSION The optimized method is stable, reliable and simple, which can be used for extraction and antioxidant activity determination of β-asarone from Acori Tatarinowii Rhizoma, and provides a basis for the further development of Acori Tatarinowii Rhizoma.

OBJECTIVE To research the chemical components of Mongolian medicinal material Gentiana veitchiorum. METHODS Separation and purification were conducted using silica gel column chromatography, Sephadex LH-20 gel column chromatography, and preparative HPLC, and the compound structure was identified through spectral data and physicochemical constants. RESULTS Ten compounds were obtained from the separation of Gentiana veitchiorum. The compounds were respectively authenticated as 2,3-dihydroxybenzyl alcohol β-glucopyranoside(1), gentiopicroside(2), 2'-(O, m-Dihydroxybenzoyl) sweroside(3), isoorientin(4), isoorientin-3'-methyl ether(5), isovitexin(6), isoorientin-4’-O-glucopyranoside(7), isosoapin(8), ursolic acid(9), β-Sitosterol(10). CONCLUSION The compound 1 is authenticated as the new benzyl alcohol glycoside. The compound 10 is firstly separated from this medicinal plant.

OBJECTIVE To prepare meloxicam solid dispersions tablets, and to investigate their dissolution in vitro. METHODS Crystal inhibition experiments were carried out to screen the carrier materials, and the solid dispersion was characterized by X-ray diffraction(XRD) amd differential scanning calorimeter(DCS). The improved bioavailability of solid dispersions was evaluated through in vivo pharmacokinetic studies. The optimum preparation process of meloxicam solid dispersion tablets was investigated, and the in vitro dissolution curve similarity factor f2 was used as the main evaluation index to screen and optimize the dosage of pH regulator, filler, disintegrator, lubricant, flow aid and the mixing time in the prescription. RESULTS The solid dispersion prepared with Kollidon@VA64 as carrier effectively maintained the supersaturated state of the drug in solution. The results of XRD and DSC showed that the crystal state of meloxicam in the solid dispersion was completely transformed into amorphous state. Compared with meloxicam, solid dispersions significantly increased the solubility, and its peak blood concentration(Cmax) and relative bioavailability were increased by 208.09% and 241.78%, respectively. The optimal formulation and process of meloxicam solid dispersion tablets prepared by direct powder pressing method were meloxicam solid dispersion 35.2%, lactose∶microcrystalline cellulose =1∶1.5, sodium citrate 9.8%, crosslinked povidone 8%, magnesium stearate 0.75%, silica 0.8%, and mixing time 5 min. The dissolution similarity factor f2 of the prepared meloxicam solid dispersion tablets and the original reference preparation in different pH medium was above 50. CONCLUSION Meloxicam solid dispersible tablets are prepared by hot melt extrusion and powder pressing method. The dissolution and bioavailability of meloxicam are improved, and the dissolution behavior of meloxicam is similar to that of the original reference preparation.

OBJECTIVE To screen the prescription and preparation method of Bupleurum nanoemulsion, and evaluate its quality, study the antipyretic effect. METHODS The emulsifier and co-emulsifier of the nanoemulsion were preliminarily screened, and then the prescription was screened by pseudo-ternary phase diagram. The quality evaluation of the appearance, particle size distribution, structure type, stability and content of the prepared Bupleurum nanoemulsion was performed. Wistar rats were further randomly divided into blank control group, model control group, positive control group(aspirin group), Bupleurum nanoemulsion high-dose, medium-dose and low-dose groups(18.00, 9.00, 3.00 g·kg−1). Except for the blank control group, the pathological model of fever rats was prepared in the other groups. According to the scheduled experimental requirements, rats in each group were given the corresponding drugs. And the temperature changes of rats in each group were recorded at 0.5, 1, 1.5, 2, 3 h to observe the antipyretic effect of Bupleurum nanoemulsion. RESULTS The best prescription of Bupleurum nanoemulsion: Tween-80 6 g and n-butanol 3 g, Bupleurum extract dissolved in pure water as water phase 20 mL, Bupleurum oil as oil phase 2 g. At room temperature, the Bupleurum nanoemulsion was a yellow-brown clear and transparent liquid, O/W nanoemulsion, with an average particle size of (77.21±3.66)nm, polydispersity index of 0.28±0.04, Zeta potential of (–18.81±1.42)mV, and saikosaponin content of 3.071 mg·mL−1, with good stability. In animal experiments, compared with the model control group, the rectal temperature of aspirin group and Bupleurum nanoemulsion high-dose group was significantly lower after the first administration(P<0.01), the rectal temperature of Bupleurum nanoemulsion middle-dose group was significantly lower after the first administration 2, 3 h(P<0.01). CONCLUSION The Bupleurum nanoemulsion is transparent and stable, and it has good antipyretic effect on fever rat model.

OBJECTIVE To establish an HPLC method for investigating the stability of mandelonitrile in commonly used solvents and quantitation determination of mandelonitrile in Jian’er Qingjie mixture. METHODS The assay was performed on an Agilent TC-C18(250 mm×4.6 mm, 5 μm) column with a mobile phase consisting of acetonitrile-0.1% phosphoric acid(23∶27) pumped at a flow rate of 1.0 mL·min–1. The column temperature was 30 ℃ and the detection wavelength was set at 207 nm. The stability of the mandelonitrile solution prepared with solvents such as methanol, 95% ethanol, acetonitrile, water, phosphoric acid solution with pH 2.0−6.0, and acetonitrile solution containing 1.0% glacial acetic acid was investigated using the peak reduction rate as the indicator. RESULTS Mandelonitrile was labile in methanol, 95% ethanol or water and relatively stable in acetonitrile. The standard solutions of mandelonitrile prepared with phosphoric acid solutions at pH 2.0−3.5 or acetonitrile containing 1.0% glacial acetic acid were stable in 12 h. The linear range of mandelonitrile was 1.033−294.987 µg·mL–1(r=0.999 9) and the average recovery was 97.4% with RSD of 0.6%(n=9). The content range of mandelonitrile in 16 batches of Jian’er Qingjie mixture produced by 5 manufactures was 3.854−154.578 µg·mL–1. CONCLUSION The established method is simple and accurate. It can be used for the quality control of Jian’er Qingjie mixture. For almond aromatic water and its preparations, the influence of solvent on stability of mandelonitrile should be noticed.

OBJECTIVE To analyze the impurities in cetirizine hydrochloride oral solution, and explore the existing problems of the production process, and provide a reference for improvement of the product quality. METHODS The related substances of 3 manufactures’ cetirizine hydrochloride oral solution were determined by HPLC. The main impurities were studied qualitively and quantitatively. The chromatographic separation was performed on a CAPCELL PAK C18 (4.6 mm×250 mm, 5 μm) column with a mixture of acetonitrile-water(17 : 83)(phosphoric acid adjusted to pH 1.5) and acetonitrile-water(35 : 65)(phosphoric acid adjusted to pH 1.5) as mobile phase by gradient elution. Detection wavelength was set at 230 nm. The confirmatory structure of the main impurities was determined by chromatography-mass spectrometry, the compatibility test between raw materials and pharmaceutical excipients was established to determine the pathway of impurities. The chromatographic separation was performed on an ACQUITY UPLC HSS-C18(150 mm×2.1 mm, 1.7 μm) column with 20 mmol·L–1 ammonium acetate(with 0.1% acetic acid)-methanol as mobile phase by gradient elution. RESULTS There might be 5 impurities in cetirizine hydrochloride oral solution. The two main related substances detected in cetirizine hydrochloride oral solution from 3 enterprises were cetirizine propylene glycol esters(a pair of diastereomers) and cetirizine glycerides(a pair of diastereomers). The emergence of impurities was highly relater to the formulation process. CONCLUSION The formulation technology of cetirizine hydrochloride oral solution need to be improved, and the active ingredients are incompatible with excipients. The related substances of cetirizine hydrochloride oral solution should be controlled from formulation design to improve the quality.

OBJECTIVE To analysis the structures of the impurities in aciclovir tablets and the compulsory degradation samples by high performance liquid chromatography coupled with hybrid quadrupole orbitrap mass spectrometry technology (HPLC-Q-Exactive Orbitrap-MS). METHODS The HPLC separation was carried out on a Waters Xbridge BEH Shield RP18 (4.6 mm×250 mm, 5 μm) by the gradient elution with a mobile phase consisting of 10 mmol·L–1 ammonium formate solution (0.15% formic acid)(A) and 10 mmol·L–1 ammonium formate solution(0.15% formic acid)-acetonitrile(50∶50)(B), and the detection wavelength was 254 nm. The Q-Exactive Orbitrap-MS was used to determine the precise first-order molecular weight and second-order fragment ions of these impurities, and the structures were identified. RESULTS Aciclovir and its impurities were well separated, and 8 major impurities with content>0.1% were detected and identified in aciclovir tablets and the compulsory degradation samples. Among them, 4 were the impurities listed in the European Pharmacopeia 10.0, and the others were unknown impurities identified for the first time. CONCLUSION The LC-MS/MS method can effectively identify the impurities in aciclovir tablets, which is significant for the production process optimization and quality control.

OBJECTIVE To conduct a rapid qualitative study on the chemical constituents of the methanol extract in Thamnolia subuliformis (Ehrh.) W.Culb. by UHPLC-Q-Exactive Focus-MS/MS. METHODS The chromatographic separation was performed on a Waters Acquity UPLC BEH C18(2.1 mm×50 mm, 1.7 μm) column with acetonitrile(A)-0.1% formic acid aqueous solution(B) as mobile phase for gradient elution, the flow rate was 0.3 mL·min–1 and the column temperature was 30 ℃. Mass spectrometry was performed using an electrospray ionization and data was collected in negative ion modes, and the detection range was m/z 80−1 200. The chemical constituents in Thamnolia subuliformis (Ehrh.) W.Culb. were identified rapidly and comprehensively based on the accurate relative molecular and combined with literature data and reference substances. RESULTS A total of 39 chemical constituents were speculatively identified, including 9 mono-substituted phenyl rings, 11 depsides, 5 depsidones, 2 dibenzofuran, 10 lipids, and 2 others. CONCLUSION The chemical constituents in the Thamnolia subuliformis (Ehrh.) W.Culb. can be identified accurately and rapidly by this method. Among them, 3 compounds(β-resorcylic acid, usnic acid, atranorin) are unambiguously identified by comparing with reference standards, 19 compounds are found from Thamnolia subuliformis (Ehrh.) W.Culb. for the first time. This paper can provide the important basis for study on pharmacodynamic material and substitute development of Thamnolia subuliformis (Ehrh.) W.Culb..