Objective The aim of this study was to develop a method for the determination of nine vulcanizing agents and accelerators in pharmaceutical rubber stoppers by headspace gas chromatography with sulfur chemiluminescence detector(HS-GC-SCD).Methods A DB-1 capillary column(30 m×0.32 mm×0.25 μm)was used with He as the carrier gas.The injection port temperature was 220 ℃,the split ratio was 10∶1,and the carrier gas flow rate was 1.5 mL·min-1.The temperature program was as follows:the starting temperature was 40 ℃,and it was increased to 60 ℃ at a rate of 5 ℃ per minute,and then to 260 ℃ at a rate of 15℃per minute.SCD detector parameters:base temperature was 280℃,combustion chamber temperature was 800 ℃,air flow rate was 60 mL·min-1,and hydrogen flow rate was 40 mL·min-1.Results The sample pretreatment method was simple and convenient,and it effectively reduced the extraction loss.The methodological results showed that all sulfides showed good linear relationships within the concentration range(r2≥ 0.990).The RSD was less than 2％;and the average recovery rate was 86.4％-97.5％.From the analysis of the sample test results,free sulfur is commonly found in rubber stoppers.Among all the samples of the vulcanization system,the free sulfur detected in the sulfur vulcanization system is higher than the free sulfur produced by degradation of other vulcanization systems.Conclusions This method is simple to operate,compared with other existing detection methods.HS-GC-SCD has a smaller matrix effect,higher sensitivity and selectivity,and is appropriate for quantifying the concentrations of sulfide present in various rubber stoppers.

Objective The aim of this study was to develop a method for the determination of nine vulcanizing agents and accelerators in pharmaceutical rubber stoppers by headspace gas chromatography with sulfur chemiluminescence detector(HS-GC-SCD).Methods A DB-1 capillary column(30 m×0.32 mm×0.25 μm)was used with He as the carrier gas.The injection port temperature was 220 ℃,the split ratio was 10∶1,and the carrier gas flow rate was 1.5 mL·min-1.The temperature program was as follows:the starting temperature was 40 ℃,and it was increased to 60 ℃ at a rate of 5 ℃ per minute,and then to 260 ℃ at a rate of 15℃per minute.SCD detector parameters:base temperature was 280℃,combustion chamber temperature was 800 ℃,air flow rate was 60 mL·min-1,and hydrogen flow rate was 40 mL·min-1.Results The sample pretreatment method was simple and convenient,and it effectively reduced the extraction loss.The methodological results showed that all sulfides showed good linear relationships within the concentration range(r2≥ 0.990).The RSD was less than 2％;and the average recovery rate was 86.4％-97.5％.From the analysis of the sample test results,free sulfur is commonly found in rubber stoppers.Among all the samples of the vulcanization system,the free sulfur detected in the sulfur vulcanization system is higher than the free sulfur produced by degradation of other vulcanization systems.Conclusions This method is simple to operate,compared with other existing detection methods.HS-GC-SCD has a smaller matrix effect,higher sensitivity and selectivity,and is appropriate for quantifying the concentrations of sulfide present in various rubber stoppers.

Fifty-nine patients (62 cases ) with chronic antritis were operated by Caldwell-Luc's operation with middle meatal antrostomy and followed up for 0.5 ~5 years. It was found that curative effect of the oper ation was quite well. Eghty patients treated with Caldwell-Lucs operation were followed up as control at the same time. Caldwell-Luc's operation with middle meatal antrostomy was found safe, easy to operate and not injurious to agger nasi, as well as partially recoverable to sinus function.

Objective:To study the effects of LSPC on impairment of learning and memory in mice induced by scopolamine and alcohol,and its possible mechanism.Method:One hundred male Kun-Ming mice were randomly divided into 2 batches,50 in each.Each batch was then divided into 5 groups(n=10):control,model,LSPC of 22.5,45,90 mg/kg bw.Group 3-5 was treated with lotus seedpod procyanidins(LSPC,dissolved in normal saline,22.5,45,90 mg/kg bw)by ig.each day for 20 d,while group 1-2 was treated with ig.normal saline.The model of learning and memory impairment was established by ip.3 mg/kg bw scopolamine hydrobromide or ig.40% alcohol in 0.1 ml/10 g bw respectively.Then,effect of LSPC on learning and memory in mice were tested by Y-maze.As to the mice whose learning and memory ability was impaired by alcohol,their brains were dissected out after Y-maze experiment for detecting the level of MDA,the activity of SOD and MAO-B.Results:The learning and memory abilities of mice impaired by scopolamine were remarkably improved after22.5 and 90mg/kg bw LSPC treatment.In the alcohol experiment,the impairment was significantly improved after three different doses of LSPC administration.The level of MDA was reduced,the activity of SOD increased and the activity of MAO-B decreased in mice that learning and memory was impaired by alcohol.Conclusion:LSPC can improve learning and memory abilities of the mice impaired by alcohol and scopolamine,and the mechanism in alcohol experiment probably lay on its suppressive effect on MAO-B activity and protection of neurons from oxidative stress.