高效液相色谱法同时测定小儿解表颗粒中8种成分的含量及主成分分析_刘宏明
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高效液相色谱法同时测定止颤颗粒中芒果苷和芍药苷的含量吴飞;洪燕龙;张继全;阮克锋【摘要】目的建立高效液相色谱法(HPLC)用于同时测定止颤颗粒中芒果苷和芍药苷的含量.方法色谱柱为Agilent Zorbax SB C18(4.6 mm×250 mm,5μm),流动相为乙腈-0.2%冰醋酸溶液(15∶85),流速1.0 mL· min-1,柱温30℃,检测波长230nm.结果芒果苷和芍药苷的进样质量分别在0.05340~2.670μg(r =0.9999)和0.02930 ~1.465μg(r =0.9997)范围内线性良好,平均加样回收率分别为99.88%(RSD=1.6%)和99.78%(RSD=1.2%).结论该研究建立的方法专属性强、重复性好、结果准确可靠,可用于止颤颗粒的质量控制和评价方法.%Objective To establish a HPLC method for the simultaneous determination of mangiferin and paeoniflorin in Zhichan granules.Methods The separation wa s carried on an Agilent Zorbax SB C18 column (4.6 mm × 250 mm,5 μm) and acetonitrile-0.2%acetic acid solution (15∶85) was employed as the mobile phase.The flow rate was 1.0 mL · min-1 with UV detection wavelength at 230nm and the column temperature was kept at30 ℃.Results The linear ranges of mangiferin and paeoniflorin were0.05340 ~2.670μg (r =0.9999) and 0.02930 ~1.465 μg (r=0.9997),respectively.The average recoveries were 99.88% (RSD =1.6%) and 99.78% (RSD =1.2%).Conclusions The method is simple and accurate with good specificity and reproducibility,and it can be used for the quality control and evaluation of Zhichan granules.【期刊名称】《安徽医药》【年(卷),期】2016(020)012【总页数】4页(P2266-2269)【关键词】止颤颗粒;芒果苷;芍药苷;高效液相色谱法;含量测定【作者】吴飞;洪燕龙;张继全;阮克锋【作者单位】上海中医药大学中药学院,上海 201203;上海中医药大学中药现代制剂技术教育部工程研究中心,上海 201203;上海张江中药现代制剂技术工程研究中心,上海 201203;上海中医药大学中药现代制剂技术教育部工程研究中心,上海201203;上海张江中药现代制剂技术工程研究中心,上海 201203;上海中医药大学中药现代制剂技术教育部工程研究中心,上海 201203;上海张江中药现代制剂技术工程研究中心,上海 201203;上海中医药大学中药现代制剂技术教育部工程研究中心,上海 201203;上海张江中药现代制剂技术工程研究中心,上海 201203【正文语种】中文止颤颗粒来自于上海市中医医院的临床有效经验方,具有益气养阴、熄风清热的功效,主要用于肝肾不足、气血两虚型帕金森病的治疗,能有效改善震颤、肢体僵硬、便秘等症状,无论是单用还是与西药合用,临床效果均较好[1-5]。
基金项目:上海市卫生局中医药科研基金(编号:2012G003A )上海市教委优秀青年教师基金(编号:ZZjdyx13092)通讯作者:唐跃年 Tel :(021)25077162 E-mail :tyn2018@高效液相色谱质谱联用法测定射干合剂中8种中药成分的含量林志燕1 杨荣富2 唐跃年1 (1.上海交通大学医学院附属新华医院 上海200092;2.上海计划生育科学研究所)摘 要 目的:建立一种高效液相色谱质谱联用法同时测定黄芩苷、野黄芩苷、汉黄芩素、咖啡酸、麻黄碱、射干苷、次野鸢尾黄素、黄芩素等8种中药成分的含量及其在我院自有制剂射干合剂中的应用。
方法:色谱条件:色谱柱为ZORBAX SB-C 18(2.1mm ˑ50mm ,1.8μm ),流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,流速为0.3ml ·min -1,柱温:35ħ;质谱条件:采用电喷雾离子源(ESI ),多反应离子监测(MRM ),结合正负离子扫描切换,其中咖啡酸、野黄芩苷、射干苷采用负离子模式检测,黄芩苷、汉黄芩素、次野鸢尾黄素、黄芩素、麻黄碱采用正离子模式检测。
结果:黄芩苷、野黄芩苷、汉黄芩素、咖啡酸、麻黄碱、射干苷、次野鸢尾黄素、黄芩素的定量限分别为1.44ˑ10-4,4.20ˑ10-3,2.95ˑ10-4,7.80,4.90ˑ10-3,4.6ˑ10-2,3.18ˑ10-4,4.85ng ·ml -1,检测限分别为4.32ˑ10-5,1.3ˑ10-3,8.84ˑ10-5,0.77,2.90ˑ10-4,3.33ˑ10-4,9.5ˑ10-5,1.46ng ·ml -1;在相应的线性范围内R 2>0.9923;日内和日间精密度(RSD )均小于5%,平均回收率均在80%~120%。
结论:本方法在20min 内实现这8种化合物的分离和测定,简单、快速、灵敏、准确,可用于射干合剂多成分含量测定。
高效液相色谱法测定小儿咳喘灵冲剂中麻黄碱的含量
林月英;李红梅;窦国义
【期刊名称】《天津药学》
【年(卷),期】2004(16)4
【摘要】目的:建立高效液相色谱法测定小儿咳喘灵冲剂中麻黄碱的含量.方法:采用phenomenex C18柱(4.6 mm×250 mm,5μm),流动相为0.01 mol/L磷酸二氢钾溶液(用磷酸调pH至2.40)-甲醇(92:8),流速1.00ml/min,检测波长210 nm.结果:盐酸麻黄碱进样量为0.084~0.672μg范围内呈良好的线性关系(r=0.999 0),平均回收率104.2%,RSD为2.32%.结论:本法简便、准确、重复性好,可用于该制剂的质量控制.
【总页数】2页(P18-18,29)
【作者】林月英;李红梅;窦国义
【作者单位】天津市大港区药品检验所,天津,300270;天津市大港区药品检验所,天津,300270;天津市大港区药品检验所,天津,300270
【正文语种】中文
【中图分类】R972.2
【相关文献】
1.高效液相色谱法测定麻杏口服液中盐酸麻黄碱及盐酸伪麻黄碱的含量 [J], 张敏新;黄爱文;宋洪涛
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因版权原因,仅展示原文概要,查看原文内容请购买。
高效液相色谱法测定小儿氨酚烷胺颗粒中对乙酰氨基酚的含量闫海燕【期刊名称】《化学与生物工程》【年(卷),期】2011(28)6【摘要】A method for determination of content of paracetamol in Child Pediatric Paracetamol and Amanta-dine Hydrochloride Granules by HPLC was established. The separation was performed on a column of Eclipse XDB-C18(4. 6 mm×150 mm, 5 μm) , with methanol : water(40: 60) as mobile phase at a flow rate of 1. 0 mL · min-1. The detection wavelength was 275 nm and the injection volume was 20 μL. The results showed that paracetamol of 5. 84 - 58. 4μg · mL-1 had a good linear relationship,the regression equation for paracetamol was ;y = 20. 96x+0. 8787,R2=0. 9998, the average recovery was 103. 3%,RSD=3. 57%. This method is convenient, accurate, and reproducible. Therefore, it can serve as a novel way to determine the content of paracetamol in Child Pediatric Paracetamol and Amantadine Hydrochloride Granules.u0000 999%建立了高效液相色谱法测定小儿氨酚烷胺颗粒中对乙酰氨基酚的方法。
HPLC同时测定感冒解毒灵颗粒中8种有效成分的含量张 娟1,杜 武2,张秋芳1,刘宏明1*(1. 淄博市食品药品检验研究院,山东淄博 255086;2. 淄博市中心医院,山东淄博 255036)摘要:目的建立高效液相色谱法同时测定感冒解毒灵颗粒中(R, S)-告依春、新绿原酸、绿原酸、升麻素苷、5-O-甲基维斯阿米醇苷、橙皮苷、连翘苷和牛蒡苷8种有效成分的含量。
方法采用Synergi TM Hydro-RP 80 Ȧ色谱柱(250 mm×4.6 mm,4 μm),流动相为乙腈-0.1 %磷酸(梯度洗脱),流速为1.0 ml/min,柱温35 ℃。
结果 8种成分分离良好;各成分的进样质量范围分别在0.5485~21.94 ng(r=0.9998)、8.070~322.8 ng(r=0.9998)、19.67~786.8 ng(r=0.9999)、20.89~835.8 ng(r=0.9999)、6.400~256.0 ng(r=0.9996)、163.3~6531 ng(r=0.9998)、48.02~1921 ng(r=0.9999)、33.00~1320 ng(r=0.9998)范围内与峰面积呈良好的线性关系;加样回收率分别为99.76 %,99.43 %,99.90 %,97.84 %,99.62 %,99.25 %,98.67 %,98.10 %,RSD 分别为1.80 %,1.04 %,1.59 %,1.77 %,1.73 %,0.58 %,1.49 %,1.50 %。
结论此法简单、快速、灵敏、准确,可用于同时测定感冒解毒灵颗粒8个指标性成分。
关键词:高效液相色谱法;感冒解毒灵颗粒;(R, S)-告依春;新绿原酸;绿原酸;升麻素苷;5-O-甲基维斯阿米醇苷;橙皮苷;连翘苷;牛蒡苷;含量测定中图分类号:R917 文献标识码:A 文章编号:1672-979X(2020)05-0395-06DOI:10.3969/j.issn.1672-979X.2020.05.012Simultaneous Determination of Eight Components in Ganmao Jieduling Granules by HPLC ZHANG Juan1, DU Wu2, ZHANG Qiu-fang1, LIU Hong-ming1(1. Zibo Institute for Food and Drug Control, Zibo 255086, China; 2. Zibo Central Hospital, Zibo 255036, China) Abstract: Objective To develop an HPLC method for the simultaneous determination of (R, S)-goitrin, neochlorogenic acid, chlorogenic acid, prim-O-glucosylcimifugin, 5-O-methylvisammioside, hesperidin, forsythin and arctiin in Ganmao Jieduling Granules. Methods The chromatographic separation was performed on a Synergi TM Hydro-RP 80 Ȧ column (250 mm×4.6 mm, 4 μm) with gradient elution by acetonitrile -0.1 % phosphoric acid at the flow rate of 1.0 ml/min. The column temperature was 35 ℃. Results The ranges for linear correlation of (R, S)-goitrin, neochlorogenic acid, chlorogenic acid, prim-O-glucosylcimifugin, 5-O-methylvisammioside, hesperidin, forsythin and arctiin were 0. 5485-21.94 ng (r=0.9998), 8.070-322.8 ng (r=0.9998), 19.67-786.8 ng (r=0.9999), 20.89-835.8 ng (r=0.9999), 6.400-256.0 ng (r=0.9996), 163.3-6531 ng (r=0.9998), 48.02-1921 ng (r=0.9999) and 33.00-1320 ng (r=0.9998), respectively. The average recoveries were 99.76 %, 99.43 %, 99.90 %, 97.84 %, 99.62 %, 99.25 %, 98.67 % and 98.10 %, with RSD s of 1.80 %, 1.04 %, 1.59 %, 1.77 %, 1.73 %, 0.58 %, 1.49 % and 1.50 %, respectively. Conclusion This method is simple, rapid, sensitive and accurate, and can be used to determine the eight components in Ganmao Jieduling Granules simultaneously.Key Words:HPLC; Ganmao Jieduling Granules; (R, S)-goitrin; neochlorogenic acid; chlorogenic acid; prim-O-glucosylcimifugin; 5-O-methylvisammioside; hesperidin; forsythin; arctiin; determination收稿日期:2020-02-18作者简介:张娟,主管药师,硕士,从事药品的检验与质量标准研究工作E-mail:**********************通讯作者:刘宏明,副主任中药师,硕士,从事中药的检验与质量标准研究工作Tel:0533-*******E-mail:****************感冒解毒灵颗粒收载于《卫生部药品标准中药成方制剂》第十九册,是纯中药制剂,由紫苏叶、板蓝根、前胡、防风、金银忍冬叶、连翘、麦冬、苦杏仁、羌活、川芎、陈皮、桑白皮、牛蒡子等13味中药构成,功能主治为解表散寒,宣肺止咳,清热解毒[1]。
高效液相色谱法测定小儿清解冲剂中连翘苷含量何绍萍;陈华龙【期刊名称】《中国药业》【年(卷),期】2011(020)003【摘要】目的建立测定小儿清解冲剂中连翘苷含量的高效液相色谱法.方法采用依利特Hypersil ODS2色谱柱(200film×4.6 mm,5 μm),以乙腈-水(25:75)为流动相,检测波长278 nm,流速为1.0 mL/min.结果连翘苷进样量与峰面积的线性范围为0.103 9~0.519 5 μg(r=0.999 7),平均回收率为98.95%.RSD为0.68%(n=6).结论高效液相色谱法简便、准确、重复性好,可用于小儿清解冲剂的质量控制.%Objective To establish a determination method of forsythin in Xiaoerqingjie Granules by HPLC. Methods The determination was carried out on the Hypersil ODS2 column(200 mm ×4.6 mm, 5 μm) with the mobile phase of methanol-H2O(25:75). The detective wavelength was set at 278 nm and the flow rate was 1.0 mL/min. Results The linear range of forsythin was 0. 103 9-0. 519 5 μg( r =0. 999 7).The average recovery rate of forsythin was 98.95%, RSD was 0.68% (n=6).Conclusion This method is simple, accurate and reproducible, which is suitable for the quality control of Xiaoerqingjie Granules.【总页数】2页(P21-22)【作者】何绍萍;陈华龙【作者单位】广东省韶关市药品检验所,广东,韶关,512028;广东省韶关市药品检验所,广东,韶关,512028【正文语种】中文【中图分类】R284.1;R286.0【相关文献】1.高效液相色谱法测定小儿感冒颗粒中连翘苷含量 [J], 朱影影2.高效液相色谱法测定清热解毒冲剂中连翘苷的含量 [J], 马尔丽;季申3.反相高效液相色谱法测定小儿感冒颗粒中连翘苷含量 [J], 郑小平;杨堃4.高效液相色谱法测定小儿清咽冲剂中牛蒡苷的含量 [J], 曲英杰;李春来5.高效液相色谱法测定小儿化痰止咳冲剂中盐酸麻黄碱的含量 [J], 朱福秋;陈宗良因版权原因,仅展示原文概要,查看原文内容请购买。
HPLC法同时测定六味能消丸中8种成分的含量康慧;刘亚蓉【期刊名称】《中国药房》【年(卷),期】2017(028)024【摘要】目的:建立同时测定六味能消丸中土木香内酯、异土木香内酯、没食子酸、大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚含量的方法.方法:采用高效液相色谱法.色谱柱为DiamonsilC18,流动相为甲醇-乙腈-0.1%冰醋酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为254 nm(土木香内酯、异土木香内酯、大黄素、芦荟大黄素、大黄酸、大黄素甲醚、大黄酚)、270 nm(没食子酸),柱温为25℃,进样量为10 μL.结果:土木香内酯、异土木香内酯、没食子酸、芦荟大黄素、大黄酸、大黄素、大黄素甲醚、大黄酚检测进样量线性范围分别为0.121~3.63μg(r=0.999 9)、0.122~3.66μg(r=0.999 9)、0.219~6.57 μg(r=0.999 9)、0.016 4~0.492 μg(r=0.999 7)、0.017 3~0.519 μg(r=0.999 9)、0.015 3~0.459 μg(r=0.999 9)、0.007 2~0.216 μg(r=0.999 9)、0.016 2~0.486μg(r=0.999 9);定量限分别为0.41、0.26、0.35、0.13、0.17、0.14、0.15、0.13 ng,检测限分别为0.12、0.08、0.11、0.04、0.05、0.04、0.05、0.04 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为98.05%~102.46%(RSD=1.75%,n=6)、98.55%~102.89% (RSD=1.91%,n=6)、98.53%~102.34%(RSD=1.66%,n=6)、101.71%~103.41%(RSD=0.57%,n=6)、101.04%~103.01% (RSD=0.69%,n=6)、101.63%~102.75% (RSD=0.39%,n=6)、96.94%~101.11% (RSD=1.61%,n=6)、98.06%~99.10%(RSD=0.40%,n=6).结论:该方法准确、简便,可用于六味能消丸中8种成分含量的同时测定.%OBJECTIVE:To establish the method for simultaneous determination of alantolactone,isoalantolactone,gallic acid,emodin,aloe-emodine,rhein,physcion and chrysophanol in Liuwei nengxiaopills.METHODS:HPLC method was adopted.The determination was performed on Diamonsil C18 with mobile phase consisted of methanol-acetonitrile-0.1% glacial acetic acid (gradient elution) at the flow rate of1.0 mL/min.The detection wavelengths were set at 254 nm (alantolactone,isoalantolactone,emodin,aloe-emodine,rhein,physcion and chrysophanol),270 nm (gallic acid).The column temperature was 25 ℃,and sample size was 10 μ L.RESULTS:The linear ranges ofalantolactone,isoalantolactone,gallic acid,emodin,aloe-emodine,rhein,physcion,chrysosphanol were 0.121-3.63 μg(r=0.9999),0.122-3.66 μg(r=0.999 9),0.219-6.57 μg(r=0.999 9),0.016 4-0.492μg(r=0.999 7),0.017 3-0.519 μg(r=0.999 9),0.015 3-0.459 μg(r=0.9999),0.007 2-0.216 μg(r=0.999 9),0.016 2-0.486(r=0.999 9).The limits of quantification were 0.41,0.26,0.35,0.13,0.17,0.14,0.15,0.13 ng;limits of detection were 0.12,0.08,0.11,0.04,0.05,0.04,0.05,0.04 ng.RSDs of precision,stability and reproducibility tests were all lower than 2.0%.The recoveries were 98.05%-102.46% (RSD=1.75 %,n=6),98.55%-102.89%(RSD=1.91%,n=6),98.53 %-102.34% (RSD=1.66%,n=6),101.71%-103.41%(RSD =0.57 %,n=6),101.04%-103.01%(RSD=0.69%,n=6),101.63%-102.75%(RSD=0.39 %,n=6),96.94%-101.11% (RSD=1.61%,n=6),98.06%-99.10%(RSD=0.40%,n=6).CONCLUSIONS:The method is accurate,simple andsuitable for simultaneous determination of 8 components in Liuwei nengxiao pills.【总页数】4页(P3433-3436)【作者】康慧;刘亚蓉【作者单位】青海省人民医院药房,西宁810008;青海省药品检验检测院,西宁810016【正文语种】中文【中图分类】R927.2【相关文献】1.HPLC法同时测定六味地黄丸中4种活性成分的含量 [J], 王晓燕;黄霞;霍甜甜;李振国2.HPLC法测定六味地黄丸(浓缩丸)中丹皮酚的含量 [J], 贾瑞艳;刘影3.HPLC法测定六味地黄丸(浓缩丸)中熊果酸含量实验条件的探讨 [J], 邹宏;熊艺芬;吴铁荣;罗玲英4.HPLC法同时测定六味地黄丸中3种成分含量 [J], 段彬;魏玉辉5.HPLC法测定六味地黄丸及六味地黄胶囊中齐墩果酸、熊果酸的含量 [J], 丁晴;徐德然;王峥涛因版权原因,仅展示原文概要,查看原文内容请购买。
高效液相色谱法测定小儿热速清口服液中绿原酸、黄芩苷和葛根素许海棠;黄富嵘;廖艺【摘要】用高效液相色谱法测定一种中成药"小儿热速清"口服液中的绿原酸、黄芩苷和葛根素含量。
采用Zorbax SB-C18色谱柱分离,以不同比例混合的甲醇和乙酸-水(1+99)溶液为流动相,进行梯度洗脱,在327nm波长处测定绿原酸、黄芩苷的含量,在250nm波长处测定葛根素的含量。
绿原酸质量浓度在3.0~30.0mg.L-1范围内呈线性关系;黄芩苷质量浓度在2.7~27.0mg.L-1范围内呈线性关系;葛根素质量浓度在3.1~31.0mg.L-1范围内呈线性关系。
方法的平均回收率为99.5%,99.8%,99.3%,相对标准偏差(n=6)分别为0.88%,0.84%,1.0%。
%The effective components,i.e.chlorogenicacid,baicalin and puerarin,in a TCM preparation,named "xiao-er resuqing"oral liquor,were determined by HPLC.The Zorbax SB-C18 chromatographic column was used as the stationary phase and mixtures of methanol andCH3COOH-H2O(1+99) solution with various proportions were used in the gradient elution.UV detections at 327 nm(for chlorogenic aicd and baicalin) and at 250 nm(for puerarin) were adopted in the determinations.Linear relationships between values of peak area and mass concentration of the 3 compounds were found in the following ranges of① 3.0-30.0 mg·L-1,② 2.7-27.0 mg·L-1 and ③ 3.1-31.0 mg·L-1 respectively.Values of average recovery obtained were 99.5%(for chlorogenic acid),99.8%(for baicalin) and 99.3%(for puerarin).Valuesof R SD′s(n=6) found for the 3 compounds were 0.88%,0.84% and 1.0% respectively.【期刊名称】《理化检验-化学分册》【年(卷),期】2011(047)011【总页数】3页(P1326-1328)【关键词】高效液相色谱法;小儿热速清口服液;绿原酸;黄芩苷;葛根素【作者】许海棠;黄富嵘;廖艺【作者单位】广西民族大学化学与生态工程学院,南宁530006;广西大学化学化工学院,南宁530004;南宁市第二人民医院,南宁530031【正文语种】中文【中图分类】O652.63小儿热速清口服液是由柴胡、黄芩、板蓝根、葛根、金银花、水牛角、连翘、大黄等多味药材加工制成,具有清热解毒、泻火利咽的功效,用于小儿风热感冒、发热头痛、咽喉红肿、鼻塞流涕、咳嗽、便秘等症。
高效液相色谱法同时测定清肺抑火片中8个成分的含量叶隽,陈斌,余岳林,张少敏(上海市静安区食品药品检验所,上海200435)摘要 目的:建立高效液相色谱法同时测定清肺抑火片中栀子苷、黄芩苷、小檗碱、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚8个有效成分的含量。
方法:采用Eclipse Plus C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,流速1 mL·min-1,检测波长254 nm,柱温30 ℃。
结果:8个有效成分的线性范围:栀子苷,4.782~95.648 μg·mL-1(r=0.999 3);黄芩苷,1.449 ~28.988 μg·mL-1(r=0.999 4);盐酸小檗碱,1.625~32.498 μg·mL-1(r=0.999 7);芦荟大黄素,0.982~19.650 μg·mL-1(r=1.00 0);大黄酸,0.703~14.070 μg·mL-1(r=1.00 0);大黄素,0.535~10.710 μg·mL-1(r=1.000);大黄酚,0.945~18.900 μg·mL-1(r=1.000);大黄素甲醚,1.505 ~30.100 μg·mL-1(r=1.000)。
平均加样回收率(n=3)在98.8%~100.4%之间,RSD均在0.24%~1.3%。
8个成分的含量分别为栀子苷,0.610~0.916 mg·g-1;黄芩苷,0.249~0.374 mg·g-1;小檗碱(按盐酸小檗碱计),0.043~0.065 mg·g-1;芦荟大黄素,0.088~0.132 mg·g-1;大黄酸,0.147~0.221 mg·g-1;大黄素,0.089~0.133 mg·g-1;大黄酚,0.193~0.290 mg·g-1;大黄素甲醚,0.046~0.070 mg·g-1。