高效液相色谱法同时测定九制大黄丸中5组分含量

目的 建立同时测定九制大黄丸中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚含量的高效液相色谱(HPLC)法。方法 色谱柱为C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(77∶23),流速1.0 m L/min,检测波长254 nm,柱温40℃,进样量20μL。结果 芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的进样质量浓度线性范围分别为4.6~92μg/m L,3.8~76μg/m L,4.0~800μg/m L,5.0~100μg/m L和17.6~352μg/m L,平均回收率分别为99.38%,99.04%,99.72%,99.59%和99.52%,RSD分别为0.80%,1.02%,0.50%,0.54%,0.92%(n=6)。结论 HPLC法可同时测定九制大黄丸中5组分的含量,专属性强,分离效果好。     

高效液相色谱法测定新保肾片中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量

目的 建立新保肾片中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量测定方法,为生产质量提供保障。方法 采用高效液相色谱法测定,色谱柱为Lichrospher-C₁₈柱(250 mm ×4.6 mm,5 μm),流动相为甲醇:0.1%磷酸溶液(7030),流速为1.0 ml/min,柱温为35 ℃,检测波长为254 nm。结果 芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在2.30~18.4 μg/ml(r=1.0)、2.930~23.44 μg/ml(r=1.0)、5.00~40.0 μg/ml(r=1.0)、14.870~118.96 μg/ml (r=0.999 8)、7.410~59.28 μg/ml(r=0.999 9)范围内有良好的线性关系,平均回收率分别为100.16%、102.91%、99.76%、100.32%、100.44%,RSD分别为1.58%、1.27%、1.67%、1.33%、1.03%(n=9)。结论 该方法准确易行,便于质量控制。     

高效液相色谱法测定三黄片中蒽醌类衍生物的含量

目的建立同时测定三黄片中葸醌类衍生物含量的RP-HPLC。方法用YWG-C18反相柱(200mm×4.6mm,10μm),流动相为甲醇-0.1%磷酸溶液(90∶10),流速为1.0mL/m in,检测波长为440nm。结果本法线形关系良好,平均回收率为96.37%~101.28%,RSD 0.8%~1.08%。结论建立的定量方法可用于三黄片质量控制标准。     

高效液相色谱法测定肾衰健颗粒剂中大黄成分的含量

目的：建立肾衰健颗粒剂中大黄5种成份的含量测定方法。方法：以HPLC法测定含量，ODS柱为固定相，甲醇—0.5％磷酸(85：15)为流动相，检测波长为254nm，流速为1.0mL.min^-1。结果：平均回收率及RSD分别为芦荟大黄素91.92％，1．65％；大黄酚101．43％，2．08％；大黄素101．77％，1.57％；大黄酚100．93％，0．88％；大黄素甲醚101.09％，2.10％。结论：该方法简便易行，结果准确，重现性好，可有效地控制该制剂的质量。     

高效液相色谱法测定四消片中大黄素及大黄酚的含量

目的:建立高效液相色谱法测定四消片中大黄素及大黄酚的含量。方法:选用 KRO-MASIL C_(18)分析柱(150×4.6mm)5μm,流动相为甲醇—0.1％磷酸溶液(85∶15),检测波长254nm。结果:大黄素在4.184～41.84μg/mL(γ=0.9999,n=5),大黄酚在21.08～210.8μg/mL(γ=0.9999 n=5)浓度范围内呈线性关系,大黄素和大黄酚平均回收率分别在99.36％和99.63％(RSD 分别为0.78％和1.01％)。结果:本法可用于四消片的定量检验。     

高效液相色谱法测定妇炎消片中大黄酚和大黄素含量

目的 初步建立妇炎消片的质量标准.方法 采用高效液相色谱法测定妇炎消片中的大黄酚和大黄素的含量.色谱柱为C18柱(250mm×4.6mm,5μm),以甲醇-0.1%磷酸溶液(85:15)为流动相,流速为1.0mL/min,检测波长为254 nm.结果 大黄素和大黄酚进样量线性范围分别为0.038 1～0.476 0 μg和0.082 4～1.030 0 μg,平均回收率为98.89%和99.01%,RSD分另4为0.78%和1.09%(n=6).结论 该方法简便易行、重现性好,可有效控制该制剂的质量.     

不同厂家大黄碳酸氢钠片中大黄素、大黄酚的含量考察

目的考察8个厂家大黄碳酸氢钠片中大黄素、大黄酚的含量。方法采用高效液相色谱法,色谱柱为C18（250mm×4．60mm,5μm）,流动相为甲醇-0．1％磷酸溶液（85：15）,检测波长为254nm,柱温为35℃,流速为1．0ml／min。结果方法线性关系良好,大黄素、大黄酚含量测定的平均回收率分别为96．67％、99．90％,RSD分别为0．57％、0．84％。测定8个厂家生产的15批大黄碳酸氢钠片,结果样品中大黄素和大黄酚含量具有显著性差异。结论大黄碳酸氢钠片的现行标准不能有效控制产品质量,采用HPLC法测定大黄碳酸氢钠片中大黄素和大黄酚的含量,方法简便、准确、重现性好,可以作为大黄碳酸氢钠片的质量控制方法。     

高效液相色谱法测定决明子4种成分含量

目的建立同时测定决明子中4种成分含量的高效液相色谱(HPLC)法。方法色谱柱为迪马Dimonsil柱(150 mm×4.6mm,5μm),流动相为乙腈-甲醇-0.1%磷酸溶液(49∶7∶44,V/V/V),等度洗脱,柱温为30℃,检测波长为222 nm,流速为1.0 mL/min,进样量为10μL。结果进样量线性范围橙黄决明素为0.02464~0.2464μg(r=0.99999),大黄素为0.0174~0.174μg(r=0.99999),大黄酚为0.02956~0.2956μg(r=0.99999),大黄素甲醚为0.016~0.16μg(r=0.99998);平均回收率橙黄决明素、大黄素、大黄酚、大黄素甲醚分别为99.41%,99.51%,99.48%和99.24%,RSD分别为0.58%,0.82%,0.95%和0.90%(n=6)。结论该方法可用于决明子质量的综合评价。     

高效液相色谱法同时测定麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素的含量

目的建立麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素的含量测定方法。方法采用奥泰ALLTIMA-C18色谱柱(4.6 mm×250 mm,5μm),以甲醇(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱[0~9min,60%A;9~20 min,60%→80%A;20~45 min,80%A];流速:1.0 mL.min-1;柱温:30℃;检测波长254 nm。结果大黄素、大黄酸、大黄酚、大黄素甲醚、芦荟大黄素线性范围分别为在9.08~81.72、8.4~75.6、13.42~120.7、7.56~68.04、8.2~73.8μg.mL-1,与峰面积线性关系良好,平均回收率分别为99.1%、99.6%、99.4%、99.8%、99.2%,RSD分别为2.0%、1.8、3.2%、1.1%、1.5%。结论本方法可作为麻仁丸中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素含量测定的一种准确、灵敏、可行的方法。     

高效液相色谱法测定山庄降脂片中大黄酚的含量

目的用高效液相色谱法测定山庄降脂片中大黄酚的含量。方法采用色谱柱KromasilC18柱,以甲醇*1mL·L(?)磷酸(97:3)为流动相,检测波长254nm。结果线性范围0.114-0.76μg(r=0.9999),方法的回收率为97.13%,RSD为1.04%。结论该方法能准确可靠地进行定性、定量检测,有效地控制该制剂的质量。     

高效液相色谱法同时测定蒙药阿那日-4散中3种成分的含量

目的：建立蒙药阿那日-4散（石榴、肉桂皮、白豆蔻、荜茇）中有效成分没食子酸、桂皮醛和胡椒碱的含量测定方法。方法：采用反相高效液相色谱法以Promosil C₁₈（4.6 mm×250 nm,5μm）为色谱柱;以乙腈-1%冰乙酸水溶液为流动相,梯度洗脱;流速为1.0 mL·min^-1;柱温为30℃;检测波长为290 nm。结果：没食子酸在0.08~0.4μg·mL^-1（r=0.9998）、桂皮醛在0.56~2.81μg·mL^-1（r=0.9996）、胡椒碱在0.52~2.59μg·mL^-1（r=0.9997）范围内与峰面积呈良好的线性关系;其平均回收率（n=6）分别为99.5%（RSD=2.3%）、99.3%（RSD=2.8%）和98.5%（RSD=2.2%）;6批样品中上述3种成分平均含量范围分别为0.198~0.241,2.44~2.61,1.41~1.54μg·g^-1。结论：所建立方法操作简便、稳定可靠、专属性强、准确度及重复性较好,为蒙药阿那日-4散质量检测提供依据。     

高效液相色谱法同时测定清肺抑火丸中13种成分的含量

目的:建立高效液相色谱法(HPLC)同时测定清肺抑火丸中芒果苷、栀子苷、盐酸小檗碱、黄芩苷、汉黄芩苷、黄芩素、芦荟大黄素、汉黄芩素、大黄酸、大黄素、白花前胡甲素、大黄酚和大黄素甲醚13种成分含量。方法:采用Dikma Platisil ODS (4.6 mm×250 mm,5 μm)色谱柱,乙腈-0.1%甲酸溶液梯度洗脱,检测波长分别为238 nm (栀子苷、盐酸小檗碱),254 nm (芒果苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚),280 nm (黄芩苷、汉黄芩苷、黄芩素、汉黄芩素),321 nm (白花前胡甲素);柱温:35℃;流速:0.8 mL·min^-1。结果:芒果苷、栀子苷、盐酸小檗碱、黄芩苷、汉黄芩苷、黄芩素、芦荟大黄素、汉黄芩素、大黄酸、大黄素、白花前胡甲素、大黄酚和大黄素甲醚线性范围分别为0.231 3~23.13,1.786 8~178.68,0.900 2~90.02,4.913 5~491.35,0.899 0~89.90,0.626 9~62.69,0.213 3~21.33,0.198 8~19.88,0.157 7~15.77,0.210 7~21.07,0.326 1~32.61,0.557 8~55.78,0.235 0~23.50 μg·mL^-1;精密度、稳定性、重复性试验的RSD小于2%;平均回收率(n=6)均大于90%。结论:该方法精确可靠、操作简便快捷,可用于清肺抑火丸中各成分的同时测定。     

高效液相色谱法同时测定金花清感颗粒中14种成分含量

目的:建立高效液相色谱法(HPLC)同时测定金花清感颗粒中新绿原酸、马钱苷酸、绿原酸、咖啡酸、獐牙菜苷、连翘酯苷A、芹菜素-7-O-β-D-吡喃葡萄糖苷、黄芩苷、连翘苷、牛蒡子苷、汉黄芩苷、黄芩素、白杨素、千层纸素共14种成分的含量,为金花清感颗粒的质量控制提供参考.方法:采用Agilent-Eclipse XDB-C...     

高效液相色谱法同时测定三黄片中的蒽醌类、黄酮类及生物碱类化合物

三黄片由大黄、黄芩浸膏和盐酸小檗碱组成，来源于祖国医学中的传统有效方剂——泻心汤，原方由大黄、黄芩、黄连三味药物组成。河北邯郸制药厂于1958年在大量研究的基础上将该方由传统的汤剂改为片剂，名“三黄片”。目前，全国有近200家企业生产三黄片。该方的主要有效成分是葸醌类、黄酮类和盐酸小檗碱。这3类成分文献报道的测定方法较多：大黄素等蒽醌类的测定方法有薄层扫描法、高效液相色谱法；黄芩苷的测定方法有极谱法、薄层扫描法、高效液相色谱法；     

Simultaneous determination of tolperisone and lidocaine by high performance liquid chromatography

A reversed phase high performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of tolperisone (TP) and lidocaine (LD) has been developed. The drugs were separated on a column (4.60×250 mm²) Spherisorb ODS (5 μm) using 5.5% triethylamine in 70/30 v/v acetonitrile/water as mobile phase 0.7 ml min⁻¹and UV detection at 254 nm. The detection limits for Tolperisone hydrochloride (TP·HCl) and lidocaine hydrochloride (LD·HCl) were 0.20 ng/20 μl and 100 ng/20 μl and the quantitation limits were 0.50 ng/20 μl and 250 ng/20 μl, respectively. Linear calibration curves over the ranges of 1–10, 10–100 and 150–500 μg ml⁻¹ for TP·HCl and 10–500 μg ml⁻¹ for LD·HCl were established. Different calibration slopes were found for TP probably owing to changes in refractive index due to increase in TP concentration. The average recoveries of the added TP in the samples (TP·HCl tablets and injection liquid). A solutions spiked with standard TP·HCl were 99.9 and 99.7% with the RSD (n=11) of 0.66 and 0.67%, respectively. The average recovery of the added LD in the sample (injection) spiked with standard LD·HCl was 98.9% with the RSD (n=11) of 0.59%. The proposed method has been applied to the determination of TP·HCl and LD·HCl in commercial products available in Thailand. Comparative determination of TP by UV spectrophotometry and LD by colorimetry were also carried out. The results obtained by both methods were in good agreement of those obtained by the proposed method verified by using t-test. The proposed RP-HPLC method is simple, accurate, reproducible and suitable for routine analysis.     

Simultaneous determination of six active components in crude and processed Fructus Corni by high performance liquid chromatography

A simple and rapid HPLC method was established for simultaneously determining six active components in Fructus Corni. The six components were separated on an Agilent Zorbax Extend C(18) column (250mmx4.6mm, 5mum) and detected by diode array detector (DAD). Mobile phase was composed of (A) aqueous phosphoric acid (0.1%, v/v) and (B) acetonitrile phosphoric acid (0.1%, v/v) using a gradient elution. Analyses were performed at 30 degrees C with a flow rate of 1.0mL/min and UV detection at 218nm, 240nm and 284nm. All calibration curves showed good linear regression (r(2)>/=0.9999) within tested ranges. The LOD and LOQ were 0.11-1.69mug/mL and 1.48-16.60mug/mL, respectively. Overall intra-day and inter-day variations were less than 4.72%, and the average recoveries were 97.97-102.51% for the analytes. The developed method can be applied to the intrinsic quality control of Fructus Corni.     

Simultaneous determination of four marker components in Yukmijihwang Tang by high performance liquid chromatography/diode array detector

Simultaneous determination method of four marker components, paeoniflorin, loganin, 5-hydroxymethyl-2-furaldehyde and paeonol in traditional herbal medicine, Yukmijihwang tang, was developed to achieve rapidly and systematic quality control by high performance liquid chromatography coupled with diode array detection. To develop this high performance liquid chromatography method, C₁₈ column (5 μm, 120 Å, 4.6 mm × 150 mm) was used with gradient elution of water and methanol as mobile phase. Validation of the chromatography method was evaluated by linearity, recovery, and precision test. Calibration curves of standard components showed excellent linearity with R² > 0.9990. Limits of detection and limits of quantification were in the ranges 0.01–0.02 and 0.04–0.07 μg/mL, respectively. The relative standard deviations of data of the intra-day and inter-day experiments were less than 1.15% and 3.76%, respectively. The results of recovery test were found to range from 94.88 to 107.43% with relative standard deviation values 0.07–2.66%. The results of validation suggested that this method was very accurate and stabilized.     

Simultaneous determination of six alkaloids in ephedrae herba by high performance liquid chromatography

A new and rapid analytical method for the simultaneous determination of six EPHEDRA alkaloids (ephedrine, pseudoephedrine, norephedrine, norpseudoephedrine, methylephedrine, and methylpseudoephedrine) in Ephedrae Herba by high performance liquid chromatography (HPLC) has been developed. Recoveries of each alkaloid were 96.0-101.6% with coefficients of deviation of 1.7-3.0%. The contents of six alkaloids in three species of EPHEDRA indigenous to China are determined and reported.     

Simultaneous determination of losartan and hydrochlorothiazide in tablets by high-performance liquid chromatography

A method for the simultaneous determination of losartan potassium and hydrochlorothiazide in tablets is described. The procedure, based on the use of reversed-phase high-performance liquid chromatography, is linear in the concentration range 3.0-7.0 microg ml(-1) for losartan and 0.5-2.0 microg ml(-1) for hydrochlorothiazide, is simple and rapid and allows accurate and precise results. The limit of detection was 0.08 microg ml(-1) for losartan and 0.05 microg ml(-1) for hydrochlorothiazide.     

高效液相色谱法测定马拉韦罗片的含量

目的建立高效液相色谱法测定马拉韦罗片的含量。方法色谱柱:Shimadzu C18柱(250 mm×4.6 mm,5μm),流动相:乙腈-0.01 mol.L-1磷酸二氢钾溶液(25∶75,V/V),柱温:(35.0±1.0)℃,流速:1.0 mL.min-1,检测波长:197 nm。结果马拉韦罗的线性范围为0.1～0.5 g.L-1(r=0.999 7),平均回收率为(99.83±0.60)%(n=9)。结论本方法简便、准确,可用于马拉韦罗片的含量测定。