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Objective To establish a method for the simultaneous determination of DOX·HCl and LND. Methods HPLC was performed on Agilent 5 HC-C18（2） （4.6 mm × 250 mm, 5 µm） column. The mobile phase was methanol-0.1% TFA aqueous solution, and the gradient elution procedure were: 0 to 3 min, 65% methanol; 3 to 7 min, 65%→90% methanol; 7 to 13 min, 90% methanol; 13 to 15 min, 90%→65% methanol; 15 to 20 min, 65% methanol. The collection time was 20 min, the balance time was 3 min, the UV detection wavelengths were 205 nm and 253 nm. The flow rate was 1.0 ml/min and the column temperature was 35℃. The amount of inlet was 10 µl. Results The method was highly specific, and both DOX·HCl and LND exhibited good linearity in the concentration range of 1-40 µg/ml and 6-240 µg/ml, respectively. The two compounds’ precision, stability, and recovery satisfied the requirements of the method. Conclusion This study established a HPLC method that was suitable for the simultaneous detection of DOX·HCl and LND. This method’s high level of specificity, accuracy, and reliability .
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Objective:To establish ion chromatography(IC) method for determination of the content of sodium glycerophosphate and phosphate salts in concentrated divitamins and sodium phosphate syrup. Methods:An AG19 -HC (50 mm× 4 mm) guard col-umn and an IonPac AS18 -HC (250 mm × 4 mm) ion analysis column were used, potassium hydroxide solution was applied as the mobile phase with gradient elution,and a conductance detector was used with suppression conductometric detection. Results:Sodium glycerophosphate and phosphate could be separated well under the chromatographic conditions. The linear range was 1.054-84.35 μg ·ml-1(r=0.999 4)for sodium glycerophosphate and 0.316 8-25.35 μg·ml-1(r=0.999 8)for phosphate. The average recovery was 99.35% (RSD=1.16%,n=9) and 98.96%(RSD=2.61%,n=9), respectively.Conclusion: The method is simple, rapid and accurate,and can be used for the quality control of concentrated divitamins and sodium phosphate syrup.
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Objective:To establish a wavelength switching HPLC with gradient elution for the simultaneous determination of six active components, [(R,S)-goitrin, salvianolic acid B, tanshinone IIA, luteolin-7-glucoside, 4-hydroxyacetophenone and scoparone ] in Ganyan Kangfu pills .Methods:An Agilent TC-C18 (250 mm ×4.6 mm, 5 μm) chromatographic column was used with the mobile phase consisting of acetonitrile and 0.1％ phosphoric acid solution with gradient elution .The flow rate was 0.9 ml· min-1 , and the column temperature was 25 ℃.( R,S)-Goitrin was detected at 245 nm, salvianolic acid B and tanshinone IIA were detected at 270 nm, luteolin-7-glucoside was detected at 348 nm, 4-hydroxyacetophenone and scoparone were detected at 278 nm.The sample volume was 10 μl.Results:The linear range of (R,S)-goitrin, salvianolic acid B, tanshinone ⅡA, luteolin-7-glucoside, 4-hydroxyacetophe-none and scoparone was 1.99-49.75 μg· ml-1(r=0.9999), 18.66-466.50 μg· ml-1(r=0.9994), 2.25-56.25 μg· ml-1(r=0.9998), 2.62-65.50 μg· ml-1(r=0.9998), 2.48-62.00 μg· ml-1(r=0.9992) and 2.55-63.75μg· ml-1(r=0.9996), respectively.The average recovery was 98.42％(RSD=0.83％), 99.56％(RSD=1.04％), 97.96％(RSD=1.53％), 96.84％(RSD=0.78％), 98.10％(RSD=1.44％) and 97.82％(RSD=1.34％)(n=6), respectively.Conclusion: The method with good reproducibility is simple and accurate , which provides a new way for the quality evaluation of Ganyan Kangfu pills .
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OBJECTIVE:To establish a method for the determination of related substances in Cabazitaxel injection. METHODS:HPLC method was used. The determination was performed on Agilent Eclipse XDB-C18column with mobile phase consisted of water-acetonitrile-ethanol(gradient elution)at the flow rate of 1.0 mL/min. The column temperature was 35 ℃,and the detection wavelength was set at 230 nm. The sample size was 20 μ L. Established method was used to determine related substances in 3 batches of Cabazitaxel injection. RESULTS:The linear relationship of cabazitaxel were 0.039-11.60 μ g/mL(r=0.999 8,n=7). The detection limit was 2×10-4μg,and quantitation limit was 8×10-4μg. RSD of precision and reproducibility tests were all lower than 10.0%(n=6). The amount of single impurity in 3 batches of samples ranged 0.07%-0.08%,and total amount of impurities were 0.26%-0.29%. CONCLUSIONS:Established method is simple,accurate and reliable,can be used for the determination of related substances in Cabazitaxel injection.
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OBJECTIVE: To establish an improved reversed-phase high performance liquid chromatography method coupled with pulsed electrochemical detection for determining the related substances of netilmicin sulfate injection. METHODS: Agilent Proshell 120 SB-C18 column (4.6 mm×150 mm, 2.7 μm)and gradient elution were used. Mobile phase A was 0.2 mol·L-1 trifluoroacetic acid in 0.1 mol·L-1 sodium hydroxide solution-acetonitrile (97:3), mobile phase B was 0.1% pentafluoropropionic acid-acetonitrile (97:3), and the flow rate was 0.8 mL·min-1. A pulsed electrochemical detector was adopted, and the temperatures of detector and column were kept at 35℃. The working electrode was a gold electrode with diameter of 3 mm and a quadruple-potential waveform (QPW)was selected as detection waveform. The injection volume was 25 μL. NaOH solution of 0.8 mol·L-1 was added post-column at a flow rate of 0.3 mL·min-1. RESULTS: A total of 28 impurities could be detected and effective separation was achieved in the typical sample and most of which could not be separated in the method of Ch.P 2015. The linearity of the calibration curve for netilmicin ranged from 0.25 to 15 μg·mL-1 with a coefficient of determination equal to 0.999 1. The LOD and LOQ of netilmicin were found to be 0.25 ng and 1.25 ng, respectively. The repeatability RSD(n=6) of the single largest impurity and total impurities were 0.9% and 0.8%, respectively. The sample solution was stable within 24 h. CONCLUSION: Compared with previously published investigations, the improved method shows higher sensitivity, better separation ability and good reproducibility, especially for differentiating the origin of bulk drug for netilmicin sulfate injection, thus is more suitable for the determination of related substances of netilmicin sulfate injection.
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Objective:To develop an HPLC gradient elution method for the simultaneous determination of fangchinoline,tetrandrine,mesaconitine,aconitine and hypaconitine in Huoxue Zhentong plaster.Methods::A Dikma-C18 (200 mm×4.6 mm,5 μm) chromatographic column was adopted,the mobile phase was methanol-acetonitrile (3∶1)(A)-0.06% diaethylamin solution (B) with gradient elution at a flow rate of 1.0 ml·min-1,the detection wavelength was 280 nm for fangchinoline and tetrandrine,and 235 nm for mesaconitine,aconitine and hypaconitine.The column temperature was set at 30 ℃,and the injection volume was 10 μl.Results::There was a good linear relationship when the content of fangchinoline,tetrandrine,mesaconitine,aconitine and hypaconitine was within the range of 7.490-149.800 μg·ml-1(r=0.999 9),14.610-292.200 μg·ml-1(r=0.999 8),4.150-83.000 μg·ml-1(r=0.999 2),5.250-105.000 μg·ml-1(r=0.999 6) and 5.140-102.800 μg·ml-1(r=0.999 9),respectively.The average recovery and the corresponding RSD were 99.87%(0.49%),97.79%(1.11%),96.97%(1.75%),98.60%(1.50%) and 97.94%(0.98%)(n=6),respectively.Conclusion:An HPLC gradient elution method is successfully established for the simultaneous determination of 5 components in Huoxue Zhentong plaster.The established method is simple,accurate and reliable,which is helpful to the quality control of Huoxue Zhentong plaster.
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Objective To establish a joint wavelength switching HPLC gradient elution method for simultaneous determination of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine in Xixian Fengshi Wan. Methods A Kromasil C18 column (4. 6 mm × 250 mm, 5 μm) was used with a mobile phase A; acetonitrile-methano (2: 1) and mobile phase B: 0. 05% acetic acid solution with gradient elution. The flow rate was 1. 0 mL/min; the injection volume was 20 μL; darutoside, kirenol and darutigenol were detected at 215 nm, and fangchinoline and d-tetrandrine were detected at 280 nm. Results In the given concentration range, the linearity ranges of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine were 6. 45-129. 00 μg/mL (r=0. 999 5), 5. 61-112. 20 μg/mL (r=0. 999 9), 4. 25-85. 00 μg/mL (r=0. 999 3), 9. 19-183. 80 μg/mL (r =0.999 8), and 11. 05-221. 00 μg/mL (r=0. 999 7), respectively; and their average recoveries and RSD were 98. 73% (1. 43%), 97. 63% (1. 28%), 99. 44% (1. 29%), 98. 33% (1. 38%), and 97. 36% (1. 37%), respectively. Conclusion The established joint wavelength switching HPLC gradient elution method is simple, accurate and reproducible; it can simultaneously determine the contents of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine in Xixian Fengshi Wnn and can be used for quality control of Xixinn Fengshi Wan.
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Objective To develop an HPLC method with gradient elution for determination of lobetyolin, scopolin, scopoletin, quercetin, kaempferol and isorhamnetin in Shenqi Jiu. Methods A Shiseido C18 column (4.6 mm×250 mm, 5μm) was adopted, the mobile phase was acetonitrile (A)-0.5% acetic acid solution (B) with gradient elution at a flow rate of 1.0 ml/min, the column temperature was set at 30 ℃, the sample quantity was 20 μl, and the detection wavelengths were 269 (lobetyolin), 346 (scopolin and scopoletin) and 360 nm (quercetin, kaempferol and isorhamnetin). Results The linear ranges of above mentioned 6 ingredients in order fell within the range of 4.59-91.80 (r=0.9999), 2.62-52.40 (r=0.9996), 1.95-39.00 (r=0.9998), 3.34-66.80 (r=0.9995), 2.30-46.00 (r=0.9991), and 2.86-57.20 μg/ml (r=0.9999), respectively. The average recoveries and RSD (n=9) were 98.27% (1.33%), 97.62% (1.48%), 99.17% (0.99%), 98.50% (1.37%), 97.35% (1.35%), and 98.86% (1.70%), respectively. Conclusion The established HPLC gradient elution method can simultaneously determine the above mentioned 6 ingredients Shenqi Jiu. The method is simple, accurate, with good reproducibility. The method is helpful for the quality control of Shenqi Jiu.
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Objective:To establish an HPLC method for the simultaneous determination of triamcinolone acetonide acetonide ( TAA) and chloramphenicol in the cream. Methods:The chromatographic system consisted of a ZORBAX SB-C18 column (250 mm × 4. 6 mm, 5μm). The mobile phase consisted of methanol and phosphate buffer with gradient elution at a flow rate of 1. 0 ml·min-1, the detection wavelength was 240nm, the column temperature was ambient, and the sample size was 20 μl. Results:The calibration curve was linear for TAA and chloramphenicol within the concentration range of 6. 12-48. 96 μg·ml-1 and 62. 1-745. 2 μg·ml-1 with the recovery of 99. 7% (RSD=1. 3%, n=9) and 99. 4%(RSD=1. 0%, n=9), respectively. Conclusion: The method is sensitive, accurate and specific, and can be used to control the quality of chloramphenicol and triamcinolone acetonide acetate cream.
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Objective To develop an HPLC method with gradient elution for determination of lobetyolin,scopolin,scopole?tin,quercetin,kaempferol and isorhamnetin in Shenqi Jiu. Methods A Shiseido C18 column(4.6 mm×250 mm,5μm)was adopted, the mobile phase was acetonitrile(A)-0.5%acetic acid solution(B)with gradient elution at a flow rate of 1.0 ml/min,the column tem?perature was set at 30℃,the sample quantity was 20μl,and the detection wavelengths were 269(lobetyolin),346(scopolin and sco?poletin)and 360 nm(quercetin,kaempferol and isorhamnetin). Results The linear ranges of above mentioned 6 ingredients in order fell within the range of 4.59-91.80(r=0.9999),2.62-52.40(r=0.9996),1.95-39.00(r=0.9998),3.34-66.80(r=0.9995),2.30-46.00 (r=0.9991),and 2.86-57.20μg/ml(r=0.9999),respectively. The average recoveries and RSD(n=9)were 98.27%(1.33%),97.62%(1.48%),99.17%(0.99%),98.50%(1.37%),97.35%(1.35%),and 98.86%(1.70%),respectively. Conclusion The established HPLC gradient elution method can simultaneously determine the above mentioned 6 ingredients Shenqi Jiu. The method is simple,ac?curate,with good reproducibility. The method is helpful for the quality control of Shenqi Jiu.
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Objective:To establish a method for the determination of related substances in enoxacin gluconate injection by HPLC with gradient elution. Methods:HPLC was performed on a DiamonsilTM C18 column (250 mm × 4. 6 mm, 5 μm), the mobile phase A was 0. 025 mol·L-1 phosphonic acid solution (adjusting pH to 3. 0 with triethylamine)-methanol- acetonitrile (80∶10∶10) and the phase B was 0. 025 mol·L-1 phosphonic acid solution (adjusting pH to 3. 0 with triethylamine)-methanol-acetonitrile (350∶325∶325) with gradient elution at a flow rate of 1. 1 ml·min-1 , the detection wavelength was 269 nm and 284 nm, the injection volume was 20μl, and the column temperature was 40℃. Results:Under the HPLC conditions, the samples had good stability and separation. The calibration curve was linear within the concentration range of 19. 80 ng·ml-1-19. 80 μg·ml-1(r=0. 999 9) for 5-hydroxymethylfur-fural with the detection limit of 0. 18ng, and the average recovery was 99. 68% with RSD of 0. 12% (n=9). Conclusion:The method is accurate, sensitive, specific and reproducible, and can be used in the determination of related substances in enoxacin gluconate in-jection.
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Objective:To establish a method for the determination of related substances in erythromycin ophthalmic ointment. Methods:The extraction method was established and optimized. An HPLC gradient elution method was used for the determination of related substances in erythromycin ophthalmic ointment. Results: One step extraction with PBS (pH 7.0) - methanol(1: 1) had promising effect. After the method validation, it was proved that the method could be used to determine the related substances in eryth-romycin ophthalmic ointment. Conclusion:The method established in the paper provides a better analytical extraction and determina-tion method for the quality control of erythromycin ophthalmic ointment.
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OBJECTIVE: To establish an HPLC method for determination of the related substances of ambrisentan tablets. METHODS: Gradient elution was performed on an Agela Venusil MP C18 column (4.6 mm × 250 mm, 5 μm). The mixture of 0.02 mol · L-1 phosphate buffer (pH 3.0) and acetonitrile (62:38) was used as mobile phase A, and acetonitrile as mobile phase B. The flow rate was 1.0 mL · min-1; the detection wavelength was set at 220 nm; and the column temperature was maintained at 35℃. RESULTS: After being treated with acid, base, heat, and oxidation, ambrisentan underwent more or less degradation. The method could effectively detect the degradation products of ambrisentan; the separation of impurities was good; the method had good specificity, linearity, and durability. CONCLUSION: The proposed method can be used to separate and determine the related substances of ambrisentan tablets, and is suitable for the quality control of this drug.
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Objective: To establish a method for the determination of the related substances in pantoprazole sodium capsules. Methods:A Kromasil C18 column (250 mm × 4. 6 mm, 5 μm) was used. 0. 01 mol·L-1 monopotassium phosphate solution (adjus-ting pH to 7. 0 with phosphoric acid)-acetonitrile was adopted as the mobile phase with gradient elution. The detection wavelength was 289 nm and the column temperature was 40℃. The injection volume was 20μl and the flow rate was 1. 0 ml·min-1 . Results:Panto-prazole sodium and its degradation substances could be well separated. The limit of detection and quantification of pantoprazole sodium was 0. 16 ng and 0. 48 ng, respectively. Conclusion:The method is simple, specific and sensitive, and can be applied to determine the related substances in pantoprazole sodium.
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Objective To establish an HPLC method for the determination of artesunate in artesunate and amodiaquine hydrochloride tablets. Methods WondaSil C18-WR column was used with mobile phase consisted of acetonitrile:phosphoric acid aqueous solution(adjust pH to 3,gradient elution);wavelength was 210 nm; flow rate was 1 mL/min and the column temperature was 30℃.Results The standard curve was linear in the range of 0.2~3.2 mg/mL(r=0.9997), average recoveries were 99.0%(RSD=1.35%, n=6).Conclusion The method is accurate and sensitive, and it can be used to control the quality of artesunate and amodiaquine hydrochloride tablets.
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Objective To establish a gradient RP￣HPLC method for determining the related substances in lumefantrine. Methods The HPLC analysis was performed on an Agilent nucleosil 100￣5 C18(4.0 mm×125 mm,5 μm) column;the mobile phase was consisted of solution A,B and C,which included phosphate buffer solutions (consisting sodium hexane sulfonate,pH was adjusted to 2. 3 )￣water￣acetonitrile￣propanol with different proportion, with a gradient elution at the flow rate of 2.0 mL.min-1 , the detection wavelength was 265 nm, and the column temperature was 35 ℃ . Results An excellent separation achieved for lumefantrine from its related substances.Lumefantrine had a good linear relationship with the peak area within the range of 0.173 4-0.693 2 μg.mL-1(r= 0.999 6).The limit of determination was 0.06 μg.mL-1 . Conclusion The method is sensitive,reproducible and specific for the separation and determination of related substances in lumefantrine.
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Objective To establish a method of the dissolution test of Xinkeshu capsule and study the dissolution behavior of sodium Danshensu, protocatechuic aldehyde, salvianolic acid B and puerarin in Xinkeshu capsule.Methods Using the dissolution determination first law of Chinese Pharmacopoeia 2010 II edition, according to the dissolution test conditions in Japan′s“quality of medical drugs information set”, different Xinkeshu capsule were inspected in pH 1.2 solution,pH 4.0 acetate buffer, pH 6.8 phosphate buffer and water.The HPLC gradient elution method was adopted to determine the dissolution of sodium Danshensu,protocatechuic aldehyde,salvianolic acid B and puerarin in Xinkeshu capsule.ResuIts Dissolution of sodium Danshensu, protocatechuic aldehyde, puerarin and salvianolic acid B of Xinkeshu capsule sample from each manufacturer were in good condition, 45min dissolution were 80% and dissolution uniformity.ConcIusion The method is simple, accurate and reproducible for the dissolution determination of this capsule .
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OBJECTIVE:To establish a method for the determination of 4 flavonoids constituents in Yinqiao capsules. METH-ODS:HPLC method was adopted. The Hypersil ODS C18 column was used with the mobile phase A of methanol-water-acetic acid (10∶88∶2,V/V/V)and B of methanol-water-acetic acid(88∶10∶2,V/V/V)in gradient elution at the flow rate of 1.0 ml/min;the de-tection wavelength was 327 nm,the column temperature was 25 ℃,and the volume was 10 μl. RESULTS:There was a good linear relationship between the amount of quercetin and peak area in the range of 0.050 9-1.018 0 μg(r=0.999 8),kaempferide in the range of 0.050 2-1.004 0 μg(r=0.999 5),isorhamnetin in the range of 0.051 0-1.020 0 μg(r=0.999 4)and rutin in the range of 0.050 4-1.007 0 μg(r=0.999 8). RSDs of precision,stability and repeatability tests were <2%. The average recoveries were 100.09%(RSD=0.93%,n=9),99.83%(RSD=0.75%,n=9),100.51%(RSD=1.17%,n=9) and 101.19%(RSD=1.08%,n=9). CONCLUSIONS:The method is amount specific,stable and reproducible and can be used for the quality control of Yinqiao capsules.
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Objective:To establish an HPLC method to determine 5-amino salicylic acid (5-ASA) and its related substances in the enemas. Methods:The liquid chromatograph was equipped with a Hypersil ODS C18 column (250 mm × 4. 6 mm,5. 0 μm) with gradient elution. The mobile phase A was composed of pH 7. 5 phosphate buffer ( PBS), tetrabutyl ammonium hydroxide solution (TBAH), methanol and water (600∶50∶50∶300), the mobile phase B was composed of pH 7. 5 PBS, TBAH, methanol and water (200∶50∶300∶450). The wavelength was 208nm, the column temperature was 40 ℃ and the injection volume was 20μl. Results:5-ASA and its two degradation products could be completely separated. The concentration of 5-ASA and the corresponding peak area had a good linear relationship within the range of 1-250μg·ml-1(r=0. 999 5). The average recovery was 99. 44%(RSD=0. 94%,n=9). Conclusion:The method is simple, sensitive and reproducible, and can be used in the determination of the content and related substances in the enemas.
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OBJECTIVE: To develop a method for separating and determining the related substances in carbazochrome sodium sulfonate injection. METHODS: HPLC Gradient elution was performed on an HP-ODS Hypersil colum. The mixture of 0.01 mol·L-1 phosphate buffer (pH 3.0) and acetonitrile (94:6) was used as mobile phase A, and acetonitrile as mobile phase B. The flow rate was 1.0 mL·min-1, the detection wavelength was set at 220 nm. RESULTS: After being treated with acid, base, heat and oxidation, carbazochrome sodium sulfonate underwent more or less degradation, the degradation products could be detected by the proposed method. Among the practical carbazochrome sodium sulfonate injection and carbazochrome sodium sulfonate and sodium choloride injection samples, the thermo degradation impurities but no impurities resulted from other treatments were detected in carbazochrome sodium sulfonate injections and carbazochrome sodium sulfonate sodium chloride injections. CONCLUSION: The proposed method can be used to separate and determine the related substances in carbazochrome sodium sulfonate injection, and is suitable for the quality control of this drug.