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71.1 天麻药材HPLC指纹图谱的研究

【作者】 石上梅; 孙婕; 杜庆鹏; 田金改; 林瑞超;

【Author】 SHI Shang-mei, SUN Jie, DU Qing-peng, TIAN Jin-gai, LIN Rui-chao(National Institute for the Control of Pharmaceutical and Biological Products, Beijing 100050, China;Technical Center of Tianjin Zhongxin Pharmaceutical Group Co., Ltd. Tianjin 300122, China)

【机构】 中国药品生物制品检定所; 天津中新药业集团股份有限公司研究中心; 中国药品生物制品检定所 北京 100050; 天津 300122; 北京 100050; 北京 100050;

【摘要】 目的用高效液相色谱法建立天麻药材甲醇提取液的指纹图谱分析方法。方法采用DikmadiamonsilODSC18(4.6mm×250mm,5μm)色谱柱,乙腈-0.4%磷酸为流动相,梯度洗脱,检测波长为270nm,以天麻苷元(对-羟基苯甲醇)为参照物。结果共有16个共有峰。结论方法准确、可靠,为有效地控制天麻药材的内在质量提供了科学依据。 更多还原

【Abstract】 OBJECTIVE To establish the fingerprints analysis of the methanol extract of Rhizoma Gastrodiae by HPLC. METHODS Dikma diamonsil ODS C18(4.6 mm × 250 mm,5 μm) was used.The mobile phase consisted of acetonitrile-0.4% phosphoric acid with gradient elution. The detective wavelength was 270 nm, and p-hydroxyl benzyl alcohol was used as reference compound. RESULTS Fingerprint consisted of 16 common peaks.CONCLUSION This method is accurate, reliable and provides a scientific basis for the quantity cont... 更多还原
【关键词】 天麻; 高效液相色谱法; 指纹图谱;
【Key words】 Rhizoma Gastrodiae; HPLC; fingerprint;
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71.2 高效液相色谱法测定复方替加氟胶囊含量及其溶出度
【作者】 吴毅彦; 左文坚;

【Author】 WU Yi-yan,ZUO Wen-jian (Tianjin Municipal Institute for Drug Control,Tianjin 300070,China)

【机构】 天津市药品检验所; 天津市药品检验所 天津300070; 天津300070;

【摘要】 目的 建立一种高效液相色谱法测定复方替加氟胶囊含量及其溶出度。方法 采用Diamonsil C18柱 (5 μm ,4 .6mm×2 5 0mm) ,用冰醋酸调节甲醇 2mmol·L-1庚烷磺酸钠溶液 (10∶90 ) pH值至 3.5 0 ,抽滤后 ,每 10 0 0mL溶液加乙醚 2mL为流动相 ,流速为 1.0mL·min-1,UV检测波长为 2 80nm。结果 此方法线性关系良好 ,替加氟与尿嘧啶的平均回收率为10 0 .0 % ,10 0 .7% ,RSD为 0 .2 1% ,0 .98% (n =9)。结论 本方法简单、快速、结果准确可靠 ,为控制复方替加氟胶囊的质量提供了依据。 更多还原

【Abstract】 OBJECTIVE A HPLC method was established for the determination of tegafur and uracil in compound tegafur capsules and its dissolution.METHODS The chromatographic condition was as following:Diamonsil C 18 column (5 μm,4.6 mm×250 mm);methanol and 2 mmol·L -1 sodium sulphonate heptane solution (10∶90,adjusted pH to 3.50 by acetic acid),with 2 mL diethyl ether to 1 000 mL solution as the mobile phase.The flow rate was 1.0 mL·min -1.The wavelength of detection was 280 nm.RESULTS The mean recoveries of... 更多还原
【关键词】 高效液相色谱法; 复方替加氟胶囊; 含量测定; 溶出度;
【Key words】 HPLC; compound tegafur capsules; assay; dissolution;
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71.3 枸橼酸莫沙必利及其制剂的HPLC测定
【作者】 邵泓;


【Author】 SHAO Hong (Shanghai Institute for Drug Control,Shanghai 200233,China)

【机构】 上海市药品检验所 上海200233;

【摘要】 目的 建立枸橼酸莫沙必利及其颗粒和片剂含量测定的HPLC ,为原料和制剂的质量控制提供有效的分析手段。方法 色谱柱 :DiamonsilC18柱 ;流动相 :甲醇 水 冰醋酸 三乙胺 (6 0 0∶40 0∶0 .5∶1) ;检测波长 :2 74nm。结果 制剂中辅料和有关物质对主药无干扰 ,枸橼酸莫沙必利在浓度 39.6 2~ 35 6 .6 μg·mL-1范围内线性关系良好 ,相关系数r=0 .9999(n =5 ) ;颗粒与片剂的平均回收率 (n =6 )分别为 10 0 .2 % (RSD =0 .70 % ) ,10 0 .9% (RSD =1.1% )。结论 本法专属性强 ,准确 ,简便。 更多还原


【Abstract】 OBJECTIVE In order to control the quality of mosapride citrate and its preparations,a method for the determination of mosapride citrate and its content in granules and tablets was developed.METHOD The chromatographic column of Diamonsil C 18 was used.The mobile phase was consisted of methanol water acetic acid glacial triethylamine(600∶400∶0.5∶1).The detection wavelength was at 274 nm.RESULTS Mosapride citrate and the other components in the samples were separated completely.The relationship bet... 更多还原
【关键词】 枸橼酸莫沙必利; 原料; 制剂; 高效液相色谱法;
【Key words】 mosapride citrate; raw material; preparation; HPLC;
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71.4 “网脱Ⅰ号”口服液长期稳定性研究
【作者】 彭燕; 李冬; 王本富; 胡辉;

【Author】 PENG Yan,LI Dong,WANG Ben-fu,HU Hui(No 474 Hospital of PLA,Urumqi 830013,China)

【机构】 解放军474医院药剂科;

【摘要】 目的:对"网脱Ⅰ号"口服液的长期稳定性进行考察。方法:根据长期稳定性实验方法,检测"网脱Ⅰ号"口服液的性状、相对密度、pH值。采用HPLC法测定芍药苷和阿魏酸含量,色谱柱:Diamonsil C18柱(4.6 mm×150 mm,5μm),流动相为乙腈-0.1%磷酸(20∶80),双波长检测230 nm/320 nm,流速为1.0 mL.min-1。结果:"网脱Ⅰ号"口服液的性状、相对密度、pH值在18个月内无明显变化;芍药苷和阿魏酸分别在10~200μg.mL-(1r=0.999 6)、10~30μg.mL-(1r=0.999 3)浓度范围内线性关系良好;加样回收率分别为(100.22±1.05)%和(100.68±1.09)%。结论:"网脱Ⅰ号"口服液在18个月内质量较稳定。 更多还原

【Abstract】 Objective: To investigate the long-term stability of" No.Ⅰdetachment of retina" oral liquids.Methods: According to the guidance of China Pharmacopoeia for long-term stability test,the characteristics,relative density and pH value of" No.Ⅰdetachment of retina" oral liquid were detected.An HPLC method was used to determine paeoni? orin and ferulic acid with the Diamonsil C18 columm(4.6 mm×150 mm,5 μm),the mobile phase was a mixture of acetonitrile-0.1% phosphoric acid(20∶80).The detection waveleng... 更多还原
【关键词】 “网脱Ⅰ号”口服液; 长期稳定性;
【Key words】 " No.Ⅰdetachment of retina" oral liquid; Long-term stability;
【基金】 中国人民解放军兰州军区科研项目(LXH-2008018)

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71.5 舒郁胶囊中麻黄碱的鉴别与含量测定研究
【作者】 白林; 任韡; 陈利平;

【Author】 BAI Lin1,REN Wei1,CHEN Li-ping2(1.Department of Drug Analysis,Pharmaceutical Care of PLA General Hospital,Beijing 100853,China;2.Department of Traditional Chinese Medicine,PLA General Hospital,Beijing 100853,China)

【机构】 解放军总医院药品保障中心药检室; 解放军总医院中医科;

【摘要】 目的:建立舒郁胶囊中麻黄碱的鉴别和含量测定方法。方法:采用TLC法和HPLC法对舒郁胶囊中的麻黄碱进行定性鉴别和含量测定。色谱条件:色谱柱为Diamonsil C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.02 mol.L-1磷酸二氢钾-磷酸(50∶950∶1),流速1.0 mL.min-1,检测波长207 nm,柱温40℃,进样量10μL。结果:在舒郁胶囊的TLC中检测到麻黄碱的特征斑点,舒郁胶囊中麻黄碱的平均含量为1.133 2 mg.g-1,麻黄碱在5.0~100.0μg.mL-1范围内呈良好线性关系,r=0.999 96,平均回收率为98.96%,RSD=0.23%。结论:本方法简便可行,重现性好,可用于舒郁胶囊中麻黄碱的鉴别和含量测定。 更多还原

【Abstract】 Objective:To establish the method for identification and determination of ephedrine in Shuyu capsule.Methods:Ephedrine in Shuyu capsule was identified by TLC,and the content was determined by HPLC.A Diamonsil C18 column(250 mm×4.6 mm,5 μm) was used with a mobile phase consisting of acetonitrile-0.02 mol·L-1 potassium dihydrogen phosphate-phosphoric acid(50∶950∶1) at a flow rate of 1.0 mL·min-1,the detection wavelength was 207 nm and the column temperature was 40 ℃.The injection volume was 10 μL.... 更多还原
【关键词】 舒郁胶囊; 盐酸麻黄碱; 薄层色谱法; 高效液相色谱法;
【Key words】 Shuyu capsule; Ephedrine hydrochloride; TLC; HPLC;
【基金】 解放军总医院新药研发基金课题

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71.6 HPLC法测定箭羽糖康片中山柰酚的含量
【作者】 白林; 徐哲; 任韡;

【Author】 BAI Lin,XU Zhe,REN Wei(Department of Drug Analysis,Pharmaceutical Care of PLA General Hospital,Beijing 100853,China)

【机构】 解放军总医院药品保障中心药检室;

【摘要】 目的:建立测定箭羽糖康片中山柰酚含量的方法。方法:采用HPLC法,色谱柱Diamonsil-C18柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.1%甲酸(33:67),流速0.8 mL.min-1,检测波长258 nm,柱温45℃。结果:山柰酚色谱峰与其他色谱峰分离良好,阴性样品无干扰。山柰酚在2.076~20.76μg.mL-1范围内呈良好线性关系(r=0.999 8),样品平均回收率为100.39%,RSD为0.52%。结论:本法简便、准确、重复性好,可用于箭羽糖康片中山柰酚的含量测定。 更多还原

【Abstract】 Objective: To develop the method for quality control of kaempferol in Jianyutangkang tablet.Methods: Diamonsil-C18 column(250 mm × 4.6 mm,5 μm)was used for separation.The mobile phase consisted of acetonitrile-0.1% formic acid(33:67) with the flow rate of 0.8 mL·min-1,and the detection wavelength was set at 258 nm.Results: The kaempferol peak was separated from other peaks without interference by negative sample.The linear range of kaempferol was 2.076-20.76 μg·mL-1(r = 0.999 8).The recovery was... 更多还原
【关键词】 箭羽糖康片; 高效液相色谱法; 山柰酚; 含量测定;
【Key words】 Jianyutangkang tablet; HPLC; Kaempferol; Content determination;
【基金】 北京市自然科学基金研发攻关项目
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71.7 RP-HPLC法同时测定复方甘草酸苷片中三组分的含量
【作者】 张卫东;


【Author】 ZHANG Wei-dong(Department of Pharmacy,Beijing Military General Hospital,Beijing,100700)

【机构】 北京军区总医院药剂科;

【摘要】 目的:建立高效液相色谱法同时测定复方甘草酸苷片中甘草酸单铵盐、甘氨酸和蛋氨酸的含量。方法:采用Diamonsil C18色谱柱(150mm×4.6mm,5μm),流动相为乙腈-0.01mol·L-1磷酸溶液(40:60),流速1.0mL·min-1,甘草酸单铵的检测波长为257nm,甘氨酸和蛋氨酸的检测波长为262nm。结果:甘草酸单铵盐、甘氨酸和蛋氨酸浓度分别在50.52~505.20μg·mL-1、10.6~106.0μg·mL-1、10.4~104.0μg·mL-1范围内呈良好的线性关系;平均回收率分别为(100.32±1.35)%、(101.02±1.80)%和(100.75±1.86)%,RSD分别为1.35%、1.78%和1.85%(n=9)。结论:本法可用于同时测定复方甘草酸苷片中甘草酸单铵盐、甘氨酸和蛋氨酸的含量,方法简便,结果准确。 更多还原


【Abstract】 Objective:To establish the RP-HPLC method for determination of ammonium glycyrrhizinate,glycine and methionine in compound glycyrrhizin tablet.Methods:The column C18(150 mm × 4.6 mm,5 μm) was used.The mobile phase consisted of acetonitrile-0.01 mol·L-1 phosphate solution(40:60).The flow rate was 1.0 mL·min-1,and the detection wavelength were 257 nm and 262 nm respectively.Results:A good linear range of 50.52 ~ 505.20 μg·mL-1 for ammonium glycyrrhizinate,10.6 ~ 106.0 μg ·mL-1 for glycine and 10.4... 更多还原
【关键词】 复方甘草酸苷片; 甘草酸单铵; 甘氨酸; 蛋氨酸; 柱前衍生化; 反相高效液相色谱
【Key words】 Compound glycyrrhizin tablet; Ammonium glycyrrhizinate; Glycine; Methionine; Precolumn derivatization; RP-HPLC;

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71.8 高效液相色谱法测定海洛因依赖者尿液中的吗啡
【作者】 张枫; 孙莉; 刘丽京; 邓艳萍;

【Author】 ZHANG Feng, SUN Li, LIU Lijing, DENG Yanping (National Institute on Drug Dependence, Peking University, Beijing, 100083)

【机构】 北京大学中国药物依赖性研究所; 北京大学中国药物依赖性研究所 北京; 100083; 北京; 100083;

【摘要】 目的:建立高效液相色谱法测定海洛因依赖者尿液中的吗啡浓度。方法:尿样经酸水解后用乙酸乙酯提取,然后采用HPLC分析。仪器条件:Diamonsil(tm)钻石C18色谱柱,流动相0·012mol·L-1磷酸二氢钾-乙腈(90:10,含0·05mmol·L-1三乙胺),流速1·0ml·min-1,检测波长205nm。结果:吗啡和内标与内源性杂质分离良好;在0·050-2·000μg·ml-1浓度范围线性关系良好(r=0·9999);检测限为0·020μg·ml-1;高、中、低3种浓度相对回收率为95·3%-104·6%,日内变异(RSD)为4·0%-8·1%,日间变异为1·9%-10·7%。结论:本法简便、准确,可用于测定海洛因依赖者尿液中的吗啡浓度。 更多还原

【Abstract】 Objective: To develop a high performance liquid chromatographic method with UV detection for the determination of morphine in the urine of heroin abusers. Methods: Morphine was extracted from the urine by ethyl acetate one step extraction method after acid hydrolysis, then determined by HPLC with Diamonsil(tm) C 18 column. The mobile phase consisted of 0.012 mol·L -1 KH2PO4-acetonitrile (90:10) containing 0.5 mmol·L -1 triethylamine. The flo... 更多还原
【关键词】 高效液相色谱; 海洛因; 吗啡; 尿液;
【Key words】 HPLC; heroin; morphine; urine;
【基金】 国家重点基础研究项目资助(项目编号:2003CB515400)
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71.9 HPLC法测定清喉咽颗粒中连翘苷的含量
【作者】 史大军; 邱海蕴; 康红英;

【Author】 Shi Dajun,Qiu Haiyun and Kang Hongying(Yichang Institute for Food and Drug Control,Hubei Pvovince 443003)

【机构】 湖北省宜昌市食品药品监督检验所;

【摘要】 目的建立高效液相色谱法测定清喉咽颗粒中连翘苷的含量。方法采用Diamonsil C18色谱柱,以甲醇-水(25∶75)为流动相,流速为1.0mL.min-1,检测波长为277nm。结果线性范围为0.0496~0.2976μg,平均回收率为99.2%,RSD为0.7%(n=9)。结论本法简便、准确、重复性好,可用于该制剂质量控制。 更多还原

【Abstract】 Objective To develop an HPLC method for determining the content of phillyrin in Qinghouyan Granules.Methods A diamonsil C18 column was adopted.The mobile phase was methanol-water(25∶75) with flow rate of 1.0mL·min-1.The detection wave length was set at 277nm.Results Good linearity was obtained from 0.0496 to 0.2976μg for phillyrin;the mean recovery(n=9) was 99.2%.and RSD was 0.7%.Conclusion The method is simple and accurate with good reproducibility.It can be applied to the quality control of Qi... 更多还原
【关键词】 高效液相色谱法; 连翘苷; 清喉咽颗粒;
【Key words】 HPLC; phillyrin; Qinghouyan Granules;
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71.10 RP-HPLC法测定肛安栓中盐酸小檗碱的含量

【作者】 高辉; 徐丽华; 崔丽华;

【Author】 Gao Hui,Xu Lihua and Cui Lihua(Shandong Institute for Drug Control,Jinan 250101)

【机构】 山东省药品检验所;

【摘要】 目的采用RP-HPLC法测定肛安栓中盐酸小檗碱的含量。方法色谱柱为Diamonsil C18;流动相为乙腈-0.05mol.L-1磷酸二氢钠溶液(用磷酸调节pH值至3)(30∶70);检测波长为270nm。结果盐酸小檗碱的进样量在0.16765~0.50294μg之间与峰面积呈良好的线性关系,r=1.0000,平均加样回收率为96.62%,RSD=0.80%(n=6)。结论本方法简便、准确,可用于肛安栓中盐酸小檗碱的含量测定。 更多还原

【Abstract】 Objective To develop a RP-HPLC method for the assay of berberine hydrochloride in Gangan Suppositories.Methods Diamonsil C18 was used with acetonitrile-0.05M sodium hydrogen phosphate(adjusting the pH value to 3 with phosphoric acid)(30∶70) as mobile phase.The detection wavelength was set at 270nm.Results The linear range was 0.16765~0.50294μg(r=1.0000).The average recovery was 96.62%and RSD was 0.80%(n=6).Conclusion The method is simple and accurate.It can be used for determination of berberine... 更多还原
【关键词】 肛安栓; 盐酸小檗碱; HPLC; 含量测定;
【Key words】 Gangan Suppositories; berberine hydrochloride; HPLC; determination;
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