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Determination of N,N-dimethyl formamide in micronazed gilibenclamide capsules by gas chromatography

Chinese Pharmaceutical Journal.2001;(2):120-122.

OBJECTIVE　To determine the content of N,N-dimethyl-formamide,the residual organic volatile solvents,in micronazed gilibenclamide capsules.METHODS　Dissolved in dimethyl sulphoxide,2 μL sample solution was injected on a DB-1 (100% dimethyl-polysiloxane) sillica capillary column using nitrogen as the carrier gas.Keep the initial temperature at 150℃ for 14 min,then it was raised to 200℃ at the rate of 40 ℃*min-1,sustained for 12 min.The injection port and FID detector were 210℃ and 240℃.Under this condition,N,N-dimethyl formamide and the internal standard tetrahydrofuran were separated completeh.RESULTS　The linear range of N,N-dimethyl formamide was 35.19～28.15 μg*mL-1,and the LOD was 8.8 μg*mL-1.The precisions was 1.9%.The recovery of N,N-dimethyl formamide was 101.4%.Three batches of sample were analysed.CONCLUSION　After validation,the method was proved to be accurate,sensitive and reliable.It is quite suitable to be used in the analysis of the N,N-dimethyl formamide in micronazed gilibenclamide capsules.

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Detection of trace glutaraldehyde in the fluid from venous circuit tube by HPLC

Feifan LIU ; Xiaoping LI ; Lihua ZHANG ; Tianbiao LAN ; Siheng GUO ; Yingqun WANG

Chinese Pharmaceutical Journal.2001;(1):57-59.

OBJECTIVE　To detect the trace glutaraldehyde in the fluid from venous circuit tube of hemodialysis,a HPLC assay was developed.METHODS　20 mL fluid taken from the venous circuit tube were derived with DNPH for 3 h,then filtered and injected. Chromatography was conducted on C18 column at 29℃.The mobile phase was consisted of 60% CH3N and 40% H3PO4 with the flow rate at 1 mL*min-1, and the detetion wavelength was at 365 nm.RESULTS　The concentrations of glutaraldehyde in the fluid ranged from 14.99 to 37.40 μg.mL-1.CONCLUSION　This HPLC method is simple and accurate to detect the trace glutaraldehyde remained in the fluid from venous circuit tube.

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Determination of tanshinoneⅡA in Rujie Xiaosan tablet

Yiheng YANG ; Xiaole ZHANG ; Shuqing WANG ; Baoxia YAN

Chinese Pharmaceutical Journal.2001;(1):56-57.

OBJECTIVE　To develope an HPLC assay for the determination of tanshinoneⅡA.METHOD　C18ODS column was used.The mobile phase was consisted of MeOH-water(70∶30).The detection wavelength was at 269 nm.RESULT　The linear regression equation was Y=9725X-2584,r=0.9997.The average recovery was 98.29% with RSD=1.86%.(n=5).CONCLUSION　The method may be used for quality control.

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Studies on the quality control of Tiaogu tablet

Suhua GUO ; Xin PAN

Chinese Pharmaceutical Journal.2001;(1):53-55.

OBJECTIVE　To establish a quality standard for Tiaogu tablet.METHODS　TLC was used to make a qualitative determination for 4 drugs in the formulary.The content of bomeol was determined by GC, the contents of strychnine and brucine were determined by TLC.RESULTS　4 drugs in the formulary were determined under stable condition with high sensitivity and precise results.CONCLUSION　This study may be helpful to develop the quality standard for Tiaogu tablet.

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TLC scanning for the determination of phillyrin in Shuanghuanglian tablet

Qin LI ; Weizhong SONG ; Qingfang LIU ; Qingsong WANG

Chinese Pharmaceutical Journal.2001;(1):51-53.

OBJECTIVE　To develop an asssay for the quantitative determination of phillyrin in Shuanghuanglian tablet.METHODS　TLCS method was selected to determine the content.RESULTS　The linearity was obtained over the range of 0.31～ 1.55 μg(r=0.9996).The average recovery was 96.9% with RSD=1.49%.CONCLUSION　The results showed that this method is sensitive,simple,specific and accurate for the determination of tetrahydropalmatine in Shuang Huanglian tablet.

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Determination of astragaloside IV in the Huangqijing by HPLC-RI

Yumei CHI ; Haiying JIANG

Chinese Pharmaceutical Journal.2001;(1):49-51.

OBJECTIVE　To establish a HPLC-RI assay for the determination of astragaloside IV in the Huangqijing solution.METHODS　The column Hypersil ODS 2(4.6 mm×200 mm,5 μm) was used.The mobile phase was consisted of methanol ane water (67∶33).The flow rate was 1 mL.min-1.RESULTS　The standard curve was linear over the range of 1～5 μg with the correlation coefficient 0.9999.The average recovery was 98.1% with the RSD 2.02%(n＝6).CONCLUSION　This method was sensitive,accurate,repeatable and easy to operate.

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Determination of paeoniflorin and geniposide in Zhonggan oral liquid by HPLC

Baizhen LU ; Xinhong LI ; Jiangfeng YANG

Chinese Pharmaceutical Journal.2001;(1):48-49.

OBJECTIVE　A RP-HPLC method was establised for the determination of paeoniflorin and geniposide in Zhonggan oral liquid.METHODS　The c18 column was used.The mobile phese was consisted of CH3CN-0.1% H3PO4(15∶85).The detection wavelength was at 230 nm.RESULTS　The average recoveries were 98.78%(RSD=2.43%,n=5)for paeoniflorin and 99.60%(RSD=1.88%,n=5)for geniposide,respectively.CONCLUSION　The method was simple,rapid and accurate.

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Pharmacokinetic study of perlolyrine in rats by means of stable isotope dilution

Ganghua TANG ; Guohui JIANG ; Lianfang ZHENG

Chinese Pharmaceutical Journal.2001;(1):45-47.

OBJECTIVE　To determine the pharmacokinetic parameters of perlolyrine in rats.METHODS　The plasma concentration and pharmacokinetic parameters of perlolyrine were determined by means of GC-MS with selected ion (m/z 247 and m/z 248) and ［2-15N］perlolyrine(m/z 248) as the internal standard.RESULTS　The concentration-time profile of perlolyrine after oral administration of perlolyrine fitted a two-compartment open model.The pharmacokinetic parameters were t1/2α=0.31 h, t1/2β=4.62 h, t1/2ka=0.10 h, tmax=0.34 h, cmax=18.74 ng.mL-1,K12=0.82 h-1, K21=0.38h-1,K10=0.29 h-1,Vb=108.16 L.kg-1,AUC=98.54 ng.h.mL-1,respectively.CONCLUSION　The method is constant,sensitive and accurate.It provided a scientific basis for the clinical use of perlolyrine.

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Pharmacokinetic study of bifonazole in human

Liangqing FU ; Dezheng WU ; Chuanhuan LUO ; Rong SHU

Chinese Pharmaceutical Journal.2001;(1):43-45.

OBJECTIVE　To study the pharmacokinetics of bifonazole in healthy human,in order to evaluate the safety of bifonazole.METHODS　8 healthy volunteers were given single dose of 300 mg bifonazole solution and cream preparation respectively in a cross-over design.Blood samples were collected at the designed time,and the concentrations of bifonazole in plasma were determined by means of GC-MS(SIM) quantitative method.The pharmacokinetic parameters were calculated with the 3P87 software.RESULTS　The plasma concentration-time curves of the two preparations were fitted to two-compartment open model.The tmax of the solution and cream preparations were 2.91 h and 5.62 h,cmax 713.46 ng.mL-1 and 410.70 ng*mL-1,respectively.The cream preparations absorption,distribution and clearance was a little slower than that of the solution preparation.However,no significant difference in their AUC.CONCLUSION　Bifonazole is a safe drug,and clinical use of the solution and cream preparation in turn is suggested to improve its therapeutic efficacy.

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Effects of Panax quinquefolium 20s-protopanaxdiol saponins on the hemodynamics and cardial oxygen metabolism in dogs with acute myocardial infarc tion

Shangyu LIU ; Dayuan SUI ; Xiaofeng YU ; Zhongzhi LU ; Li WANG

Chinese Pharmaceutical Journal.2001;(1):25-29.

OBJECTIVE　To study the effects of Panax quinquef olium 20S-protopanaxdiol saponins extracted from the leaves of panax qu inque-folium (PQDS) on the hemodynamics and cardial oxygen metabolism in dogs with acute myocardial infarction (AMI).METHODS　The paramete rs of hemodynamics and cardial oxygen metabolism were determined by using the mo del of ligation of LAD in the anaesthetized open-chest dogs.RESULTS 　In dogs treated with PQDS (in a dosage of 10 and 20 mg*kg-1 iv infusion),the myocardial blood flow (MBF) was increased and coronary vascular re sistance (CVR) was decreased significantly.The heart rate (HR) was slowed.The ar terial blood pressure (ABP),left ventricular pressure (LVP),the maximum rise rat e of left ventricular pressure(+dp/dtmax),left ventricular work index (LVW I) and total periphery resistance(TPR) were reduced,whereas the stroke index(SI) and cardiac index (CI) were increased.In addition,the decreasing range of the m aximum decline rate of left ventricular pressure(-dp/dtmax) and the rising range of left ventricular end diastolic pressure (LVEDP) were reduced.Meanwhile the cardiac oxygen consumption,myocardial oxygen utilization rate and cardiac o xygen consumption index were also decreased.CONCLUSION　PQDS had protective effects on acute myocardial ischemia including improving heart fu nction,decreasing cardiac oxygen consumption and increasing myocardial blood flo w,etc.

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