Simultaneous Determination of 6 Residual Organic Solvents in Omeprazole Magnesium by Headspace GC / 中国药房

OBJECTIVE:To establish a method for the simultaneous determination of 6 kinds of residual organic solvents in Omeprazole magnesium,such as methanol,isopropanol,acetonitrile,dichloromethane,ethyl acetate and toluenein. METHODS:Headspace GC was adopted. The determination was performed on the column of DB-624 column by temperature programming. The inlet temperature was 200 ℃,and hydrogen flame ionization detector was adopted with the temperature of 250 ℃;nitrogen gas was used as carrier gas with flow rate of 2.0 mL/min;the splitting-radio was 5 : 1,and sample size was 1 mL;the headspace tem-perature was 80 ℃ and the equilibrium time was 20 min. RESULTS:The linear range were 12.56-628.00 μg/mL for methanol(r=0.9997),20.22-1011.20 μg/mL for isopropanol(r=0.9999),1.96-97.76 μg/mL for acetonitrile(r=0.9997),3.10-154.88 μg/mL for dichloromethane(r=0.9998),20.69-1034.56 μg/mL for ethyl acetate(r=0.9998),and 3.53-176.72 μg/mL for toluene(r=0.9998);the limits of quantitation were 1.00,0.91,0.47,0.93,0.41 and 0.35 μg/mL respectively;the limits of detection were 0.31,0.30,0.14,0.31,0.12 and 0.11 μg/mL respectively;RSDs of precision,stability and reproducibility tests were lower than 3%;the recoveries were 94.53%-101.29%(RSD=2.15%,n=9),97.78%-103.42%(RSD=1.77%,n=9),96.99%-105.76%(RSD=2.59%,n=9),96.83%-102.05%(RSD=1.86%,n=9),97.98%-101.13%(RSD=0.88%,n=9)and 97.80%-102.40%(RSD=1.41%,n=9). CONCLUSIONS:The method is sensitive and accurate,can be used for the simultaneous determination of 6 kinds of residual organic solvents in Omeprazole magnesium,such as methanol,isopropanol,acetonitrile,dichloromethane,eth-yl acetate and toluenein.

Content Determination of Magnesium in Esomeprazole Magnesium by Inductive Coupled Plasma Atomic E-mission Spectrometry / 中国药师

Objective:To establish a method for the content determination of magnesium in esomeprazole magnesium. Methods:The content of magnesium in esomeprazole magnesium was determined by inductive coupled plasma atomic emission spectrometry. Re-sults:The linear range was 10.0-80.0 μg·ml-1(r=0.999 8). The average recovery was 99.55% with RSD of 1.35% (n=9). The detection limit was 0. 000 75 μg·ml-1 and the quantitative limit was 0. 002 5 μg·ml-1 . Conclusion:The method is accurate, sensitive and reproducible, which can be used for the content determination of magnesium in esomeprazole magnesium.

Simultaneous determination of six alkaloids in Coptis chinensis of different regions by RP-HPLC / 中国中药杂志

A reversed-phase HPLC method for simultaneous determination of gatrorrhizine, columbamine, epiberberine, coptisine, palmatine and berberine in Coptis chinensis was developed. Analysis was carried out on an Xtimate C18 column (4.6 mm x 250 mm, 5 microm) eluted with acetonitrile-30 mmol x L(-1) ammonium bicarbonate solution (including 0.7% ammonia and 0.1% triethylamine) by gradient elution. The detective wavelength was 270 nm, the column temperature was 30 degrees C, and the flow rate was 1.0 mL x min(-1). By the above method, the linear ranges of gatrorrhizine, columbamine, epiberberine, coptisine, palmatine and berberine were 0.85-16.96 (r = 0.9997), 1.25-24.96 (r = 0.999 5), 2.05-40.96 (r = 0.999 9), 3.65-72.96 (r = 0.999 9), 2.88-57.60 (r = 0. 999 8),13.25-264.96 mg x L(-1) (r = 0.999 6), respectively. The average recoveries (n = 6) of the six alkaloids were 101.6% (RSD 1.3%),102.5% (RSD 1.5%), 100.8% (RSD 1.9%),102. 6% (RSD 1.2%), 97.80% (RSD 1.3%), 99.01% (RSD 1.5%), respectively. The determined results demonstrate that there is a significant difference in the contents of six alkaloids and total alkaloids among the tested samples. The method is accurate, reliable and repeatable for simultaneous determination of gatrorrhizine, columbamine, epiberberine, coptisine, palmatine and berberine in C. chinensis.

HPLC fingerprint chromatography of Toufengyu Dropping Pills / 中成药

AIM: To establish a method of fingerprint analysis of Toufengyu Dropping Pill(Radix angelicae dahuricae,Rhizoma chuanxiong and green tea) by HPLC. METHODS: Hypersil ODS2 C_18(4.6 mm?250 mm,5 ?m) column was used,with mixtures of 0.1%TFA solution and acetonitrile as mobile phase in a gradient mode.The flow rate was 1.0 mL/min,the column temperature was at 30 ℃,detection wavelength was at 254 nm. RESULTS: HPLC fingerprint determination with 22 common peaks gained from 10 batches of self-made Tonfengyu Dropping Pill,there were 9 components identified,including caffeine,EGCG,ferulic acid,oxypeucedanin,imperatorin,phellopterin,cnidilin,isoimperatorin and oxypeucedanin hydrate. CONCLUSION: This method is accurate,reliable and can provide more information for the quality control of Toufengyu Dropping Pills.