1.Determination of Triptolide in Compound Tripterygium Wilfordil Syrups by HPLC
China Pharmacist 2014;(2):316-318
Objective:To establish a method for the content determination of triptolide in compound tripterygium wilfordil syrups by HPLC. Methods:The samples were analyzed on a Diamonsil C18 column(150 mm × 4. 6 mm,5μm), the mobile phase consisted of methanol and water (46∶54), the flow rate was 1. 0 ml·min-1, the detection wavelength was 224 nm, and the column temperature was kept at 30℃, and the injection volume was 10 μl. Results: The linear range of triptolide was 5. 66-33. 96 μg · ml-1 ( r =0. 999 8), and the average recovery was 99. 35% with RSD of 1. 02%(n=9). Conclusion:The method is simple and sensitive with good repeatability, and can be used to control the quality of triptolide in compound tripterygium wilfordil syrups.
2.Determination of Norisoboldine in Suoquan Capsules by HPLC
Qing WEN ; Ping NIE ; Ye DING ; Jinfeng ZHENG ; Wenli LI
China Pharmacist 2014;(2):308-309
Objective:To establish an HPLC method for the determination of norisoboldine in Suoquan capsules. Methods: The chromatographic procedure with acetonitrile-water containing 0. 5% folic acid and 0. 1% triethylamine (10∶90) as the mobile phase was carried out on an Ecosil C18 HPLC(150 mm ×4.6 mm,5 μm). The flow rate was at 1.0 ml·min-1, the detection wavelength was 280nm and the column temperature was 30 ℃. Results: The linear range of norisoboldine was within 38. 56-578. 40 ng ( r =0. 999 2), the average recovery of norisoboldine was 99. 9%(RSD=1. 7%, n=6). Conclusion:The method is highly sensitive, re-liable and accurate, and can be applied in the determination of Suoquan capsules.
3.Determination of Pantoprazole Sodium for Injection by High Performance Capillary Electrophoresis
Ziyu SONG ; Dazhong DING ; Chengzhang LUAN
China Pharmacist 2014;(2):240-242
Objective:To establish a method for the content determination of pantoprazole sodium for injection by high performance capillary electrophoresis. Methods:The determination was performed on an uncoated elastic quartz capillary column, the running buff-er was 0. 01 mol·L-1 potassium dihydrogen phosphate buffer, the running voltage was 25kV,the column temperature was 25℃ and the detection wavelength was 289 nm. Results:The linear range was good within the concentration range of 20. 05-200. 51 μg·ml-1(r=0. 999 6). The average recovery was 99. 03%(RSD=0. 86%, n=9). Conclusion:The method is simple, sensitive and reproduci-ble, and can be used in the determination of pantoprazole sodium for injection.
4.Pharmacognostical Identification of Selaginellae Uncinatae Herba
Yimei LIU ; Jia LIU ; Keli CHEN
China Pharmacist 2014;(2):232-234
Objective:To pharmacognostically identify Selaginellae uncinatae Herba to provide reference for the identification and utilization of Selaginellae uncinatae Herba. Methods:On the basis of observing the characters, structure and microscopic characteris-tics of the powder, Selaginella uncinata Herba was identified by a TLC method using amentoflavone as the reference substance. The contents of total ash, acid insoluble ash and alcohol-soluble extracts in Selaginellae uncinatae Herba were detected as well. Results:The morphological identification, microscopic identification and TLC identification of the herb was respectively established. The content limits of the total ash, acid insoluble ash and alcohol soluble extract were preliminarily determined. Conclusion:The studies provide reference for the identification and quality evaluation of Selaginellae uncinatae Herba.
5.Determination of Related Substances in Norfloxacin Glutamate and Sodium Chloride Injections
Jing ZHANG ; Qingquan WANG ; Xuping LIU ; Liangfa WU
China Pharmacist 2014;(2):229-231
Objective:To detect the related substances in norfloxacin glutamate and sodium chloride injections on the basis of nor-floxacin related substances analysis method described in Chinese Pharmacopoeia 2010 edition to establish a more scientific and feasible method. Methods:HPLC was performed under the following conditions:a Diamonsil C18(2)(250 mm ×4.6 mm,5μm) column, mo-bile phase A of 0. 025 mol·L-1 phosphoric acid-acetonitrile(87∶13), phase B of acetonitrile, with gradient elution at a flow rate of 1. 0 ml·min-1 , the detection wavelength of 278nm and 262nm, the injection volume of 20 μl, and the column temperature of 25℃. Results:Under the HPLC conditions, the samples had good stability and separation. An excellent linear relationship was achieved within the range of 0. 032-3. 179μg·ml-1(r=1. 000 0),the detection limit of impurity A was 0. 159 ng,and the average recovery was 98. 3% with RSD of 0. 64%(n=9). Conclusion:Compared with the existing methods, the gradient elution method is accurate, sen-sitive, specific and reproducible, and can be used in the determination of related substances in norfloxacin glutamate and sodium chlo-ride injections.
6.Determination of Residual Organic Solvents in Nimodipine Liposomes by Headspace Gas Chromatography
Li XIANG ; Yujia ZHANG ; Shaohua CHENG ; Xiuli ZHANG ; Mengmeng LIU ; Xiaqing FANG ; Lulu WANG ; Wensheng ZHENG
China Pharmacist 2014;(2):227-229
Objective:To establish a method for determining three residual organic solvents in nimodipine liposomes. Methods:The samples were injected into a DB-624 capillary column (30 m × 0. 32 nm,1. 8 μm) by a headspace sampler and analyzed with an FID detector, the carrier gas was nitrogen, the injector temperature was 250℃, and the detector temperature was 250℃. The column temperature was programmed raised. Results:Three residual solvents, namely ethanol, acetone and acetic ether were completely sepa-rated. There was a good linearity within the experimental concentration range. The average recovery was 98. 9%,98. 5% and 99. 4%(RSD=0. 32%,1. 12%,0. 76%,n=9), respectively. The detection limits was 0. 20, 0. 18 and 0. 22μg·ml-1, respectively . Con-clusion:The method is rapid, sensitive and accurate. It can be used in the determination of residual organic solvents in nimodipine li-posomes.
7.Improved Quality Standard for Kangshiming Mixtures
Yue XU ; Feng CAI ; Qin ZHANG ; Ting HONG ; Yanfeng XU
China Pharmacist 2014;(2):218-220
Objective:To improve the quality standard for Kangshiming mixtures. Methods:The identification of Angelicae Sinen-sis Radix, Astragali Radix and Phellodendri Chinensis Cortex was carried out by TLC. The contents of puerarin and paeoniflorin in the preparations were determined by HPLC. Results:The spots displayed in TLC were clear without interference from the negative control. The linear range for puerarin was 1. 64-49. 20μg·ml-1(r=0. 999 9) and 4. 22-63. 30μg·ml-1(r=0. 999 6) for paeoniflorin. The average recovery was 99. 63%(RSD=2. 14%,n=9) and 99. 05%(RSD=2. 70%,n=9) for puerarin and paeoniflorin, respectively. Conclusion:The method is accurate, reliable and specific, and can be used in the quality control of Kangshiming mixtures.
8.Determination of Residual Formaldehyde Fumigation on the Surface of Pharmaceutical Equipments by AH-MT Method
Jie WU ; Guanghu RUI ; Renjie SONG ; Wei SHENG ; Wenjing GONG
China Pharmacist 2014;(2):330-332
Objective:To determine the residual formaldehyde fumigation on the surface of pharmaceutical equipments by AHMT method. Methods:The reaction time of AHMT was controlled in 20 min, the solution with sodium periodate was then shaken for 30 seconds and stood for 30 seconds, and then the absorbance at 550 nm was measured. Results: The linear range of formaldehyde was 0. 250~2. 495 μg·ml-1. The recovery of formaldehyde on glass plate, color steel plate and stainless steel plate was (83. 42 ± 1. 48)%(n=3), (83. 63 ± 1. 94)%(n=3)and (83. 94 ± 2. 28)%(n=3), respectively. Conclusion:The method is proved to be convenient and accurate, and is suitable for the determination of formaldehyde on the surface of pharmaceutical equipments.
9.Analysis of Measurement Uncertainty in Determination of Irbesartan Tablets by HPLC
China Pharmacist 2014;(2):326-328
Objective:To find out the impacting factors in uncertainty by analyzing the measurement uncertainty in the determina-tion of irbesartan tablets by HPLC and provide the evidence for the measurement evaluation. Methods:A mathematic model for calcu-lating uncertainty was established, and every component in the uncertainty was assessed. Results:The expanded standard uncertainty for the HPLC determination was 2. 4%. Conclusion:The measurement uncertainty of the experiment is mainly caused by the measur-ing method.
10.Determination of Salvianolic Acid B in Ansheng Yizhi Capsules by HPLC
Huiping MA ; Lanru LI ; Zhicheng DONG ; Lei HE ; Zhengping JIA
China Pharmacist 2014;(2):314-316
Objective:To establish an HPLC method for the content determination of salvianolic acid B in Ansheng Yizhi cap-sules. Methods:A Hypersil ODS2 C18 column(150 mm × 4. 6 mm,5 μm) was used and methanol-water-formic acid (40∶60∶1) was used as the mobile phase. The detection wavelength was at 286 nm. The flow rate was 1. 0 ml·min-1 and the sample size was 10 μl. Results:The calibration curve of salvianolic acid B was linear within the range 7. 75-77. 51 μg·ml-1(r=0. 999 6). The average re-covery was 98. 17%(RSD=1. 79%, n=6). Conclusion:The method is simple, accurate and repeatable, which can be used in the quality control of Ansheng Yizhi capsules.