美国等五国西洋参人参药材中重金属残留量分析

目的建立原子吸收分光光度法测定五国四种人参药材中的铅、镉、砷、汞、铜重金属含量。方法采用原子吸收法在324.8nm波长检测铜含量,在283.3nm波长检测铅含量,在228.8nm波长检测镉含量,另外采用原子荧光光谱法测定砷、汞的含量。结果 24批五国四种人参药材中的重金属残留量西洋参为10.581～12.025mg/kg;红参（高丽参）为12.719～14.002mg/kg。结论五国四种西洋参人参药材样品中重金属残留量均符合2005年版《中国药典》（一部）及香港特区《中成药注册申请手册》的有关重金属标准规定。     

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.     

Application of a ultra performance liquid chromatography method in the determination of DNA quality and stability

The development of plasmid DNA as a pharmaceutical requires that integrity (i.e., supercoil content) be monitored as part of quality control. The standard method of determining supercoil content is gel electrophoresis followed by staining and imaging, which is complicated by a variety of factors. Previously described chromatographic methods used to quantify supercoil content have had difficulty obtaining reliable separation of the different isoforms. Using ultra performance liquid chromatography, we have optimized buffer conditions, and utilized increased column temperatures in developing a method that allows accurate quantification of each isoform by ultraviolet detection. We found that increasing the column temperature to 55°C improved separation of the isoform peaks as well as increased the resolution of each peak. We demonstrate the utility of this method by quantifying supercoil content of samples subjected to sonication, acidification or lyophilization, and storage. Our results demonstrate that this method allows for a precise quantification of individual DNA isoforms within a heterogeneous sample.     

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.     

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。     

Simultaneous determination of dexamethasone and trimethoprim by liquid chromatography

A reverse phase high performance liquid chromatography (HPLC) method to determine dexamethasone phosphate and trimethoprim is described in this paper. The separation was made in a LichrCART(R) C18 column using an acetonitrile-NaH(2)PO(4) (10 mM) (70:30, v/v) (pH 3) buffer solution as mobile phase. The mobile-phase flow rate and the sample volume injected were 1 ml/min and 20 microliter, respectively. The limits of quantification were about 0.25 mg/l for each compound. The method was applied in synthetic mixtures and in pharmaceutical formulations. Analyses were made by preparing test (from the stock solution) method whose results were compared with those obtained by means of the standard addition method. Both methods showed similar results, and then it was proved that some pharmaceuticals claimed levels were in agreement with the obtained results by using our analytical method.     

Simultaneous determination of serum flecainide and its metabolites by using high performance liquid chromatography

Simultaneous determination of serum flecainide and its oxidative metabolites was carried out by using high performance liquid chromatography (HPLC) equipped with conventional octadecylsilyl silica (ODS) column and fluorescence detector. Flecainide and its metabolites, m-O-dealkylated flecainide (MODF) and m-O-dealkylated lactam of flecainide (MODLF) in serum were extracted with ethyl acetate. The recoveries of flecainide, MODF and MODLF were greater than 92, 93, and 60% with the coefficient of variations (CVs) less than 3.2, 5.8, and 5.3%, respectively. The calibration curves were linear at the concentration range of 50–1500 ng/mL for flecainide and 10–500 ng/mL for MODF and MODLF (r>0.999). The CVs for intra-day assay were 2.7–5.3% for flecainide, 3.0–4.2% for MODF, and 3.7–4.3% for MODLF, respectively. The CVs for inter-day assay were 7.0–8.4% for flecainide, 3.3–6.7% for MODF, and 4.4–7.7% for MODLF, respectively. This assay method can be used for assessing the metabolic ability of flecainide in the patients with tachyarrhythmia.     

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...     

Simultaneous determination of 10 major flavonoids in Dalbergia odorifera by high performance liquid chromatography

A reversed-phase liquid chromatographic method was developed for the simultaneous quantification of 10 major flavonoids, namely butin, (3R)-4'-methoxy-2',3,7-trihydroxyisoflavanone, liquiritigenin, melanettin, violanone, vistitone, formononetin, dalbergin, sativanone and medicarpin in the heartwood of Dalbergia odorifera, an important traditional Chinese medicine. Samples were extracted with 60% methanol. The optimal conditions of separation and detection were achieved on an Agilent Zorbax SB-C18 column (250 mm x 4.6 mm, 5 microm) with a gradient of acetonitrile and 0.3% (v/v) aqueous acetic acid, at a flow rate of 0.8 ml/min, detected at 275 nm. The complete separation was obtained within 55 min for the 10 target compounds. All calibration curves showed good linearity (r2>0.999) within test ranges. The assay was reproducible with overall intra- and inter-day variation of less than 3%. The mean recovery of the method was 100+/-10%, with R.S.D. less than 5%. The current assay method was considered to be suitable for the quality control of D. odorifera samples and could be readily utilized for the determination of the active principles present in this medicinal herb.     

HPLC法同时测定大豆苷元及其三个氨基甲酸酯前药的含量

目的建立了一种同时测定大豆苷元及其三个氨基甲酸酯前药的含量的高效液相色谱方法。方法选用Welch Ultimate LP-C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A),体积分数0.3%甲酸水(B),甲醇(C)进行三元梯度洗脱,流速1.0 mL·min~(-1),检测波长249 nm,柱温30℃。结果应用所建立的方法,各组分在24 min内均得到较好分离。大豆苷元(Dan)、7-缬氨酸大豆苷元氨基甲酸酯(7-P)、4′-缬氨酸大豆苷元氨基甲酸酯(4′-P)和7-4′-二缬氨酸大豆苷元氨基甲酸酯(7-4′-P)的质量浓度分别在1.003～20.06 mg·L~(-1)、1.004～20.08 mg·L~(-1)、1.002～20.04 mg·L~(-1)、1.001～20.02 mg·L~(-1)范围内与峰面积呈良好的线性相关性,平均回收率分别为100.1%、100.5%、100.1%、100.2%(n=9),RSD均小于2.0%。结论所建立的方法可用于大豆苷元及其氨基甲酸酯前药的含量测定及其化学稳定性研究。     

Simultaneous determination of amiodarone and desethylamiodarone in human plasma by high performance liquid chromatography.

A rapid, sensitive and specific reversed phase HPLC method for the simultaneous assay of amiodarone and its major metabolite desethylamiodarone in human serum has been developed. This method is suitable for pharmacokinetic studies and for monitoring of the drug and metabolite concentrations in serum of patients on both short and long-term therapy with amiodarone.     

HPLC法同时测定霉酚酸及其代谢产物的方法学研究

目的 建立测定器官移植患者血浆中霉酚酸（Mycophenolic acid,MPA）与其代谢物（霉酚酸葡萄糖苷,MPAG和霉酚酸酰基葡萄糖苷,AcMPAG）的一种新颖简单的高效液相色谱（high performance liquid chromatography,HPLC）方法.方法 以10%的偏磷酸为沉淀剂采用蛋白沉淀的方法提取血浆中的待测物,MPA的类似物（the carboxybutoxy ether of MPA,MPAC）被用作内标物质.色谱分析条件是以乙腈和磷酸缓冲液（pH2.7）作为流动相的梯度洗脱,流速1.2 mL·min-1,紫外检测波长为254 nm.结果 所有待测物基线分离好,在待测范围内与峰面积线性关系良好（r2≥0.999）,方法精密（日间和日内变异度均≤6.02%）且准确（日间和日内准确度均在92.17% ~104.78%之间）.MPA、MPAG和AcMPAG在血浆中的回收率分别超过83.11%、98.62% 和93.94%,最低检测限则分别为0.1、0.2、0.1 mg·L-1.三种物质的在酸化过的血浆中,室温放置6 h、4℃条件下放置12 h、-40℃条件下放置4周及反复冻融三次均稳定无明显降解.提取后的三种物质在进样盘中放置至12 h同样稳定无降解.结论 该方法简便、灵敏且准确,可应用于MPA与其代谢物的临床监测.     

高效液相色谱法同时测定普那布林原料药中9种有关物质

摘要：目的 建立普那布林原料药中有关物质的检测方法。方法 采用高效液相色谱法,色谱柱YMC-Pack Pro C18（250×4.6 mm,5 μm）;以乙腈为流动相A,0.1%乙酸水溶液为流动相B;流速为1.0 mL·min-1梯度洗脱;检测波长为254 nm和365 nm;进样量为10 μL;柱温为35 ℃。结果 普那布林峰与各杂质峰均达到有效分离,各杂质浓度和峰面积线性关系良好,平均回收率在98.09%-108.82%。结论 本方法专属性强、灵敏、准确,可用于普那布林原料药有关物质的检测。     

高效液相色谱法同时测定帕博西尼胶囊中5种有关物质

目的采用高效液相色谱法,建立一种帕博西尼胶囊有关物质的检测方法。方法色谱柱为Ultimate XB C18(250 mm×4. 6 mm,5μm);流动相A:体积分数0. 1%三氟乙酸-水溶液,流动相B:乙腈-水-三氟乙酸(体积比70∶30∶0. 1)溶液,进行梯度洗脱;检测波长:290 nm;进样体积:10μL;流速:1. 0 m L·min~(-1);柱温:35℃;运行时间:50 min。结果杂质WB001-A、WB001-B、WB001-E、WB001-F、WB001~(-1)和帕博西尼的定量限分别为27. 0、63. 0、42. 0、26. 0、27. 0、18. 0μg·L~(-1),线性范围分别为0. 09～0. 59 mg·L~(-1)、0. 11～0. 71 mg·L~(-1)、0. 07～0. 47 mg·L~(-1)、0. 09～0. 58 mg·L~(-1)、0. 09～0. 60 mg·L~(-1)和0. 09～0. 61 mg·L~(-1),平均回收率分别为96. 79%、101. 18%、97. 23%、100. 75%和103. 56%。结论本方法可准确检测帕博西尼胶囊的有关物质。     

Simultaneous determination of bioactive marker compounds from Gardeniae fructus by high performance liquid chromatography

Gardeniae fructus is one of the medicinal herbs that have been used in Far Eastern countries, such as Korea, China, and Japan. Gardeniae fructus is the dried ripe fruit of Gardenia jasminoides Ellis (Rubiaceae) and has been used as a yellow dye. It is widely used as traditional herbal medicine for reducing fever, cholagogue, diuretic and antiphlogistic effects. We established an analytical method that was useful to evaluate the quality control, and standardize quantification monitoring of 68 samples of Gardeniae fructus collected from Korea and China. While numerous previous studies have focused on the simultaneous analysis of geniposide, which constitutes the higher proportion of Gardeniae fructus, and crocin, which determines its color, no simultaneous analysis of gardenoside and geniposide, the major components of Gardeniae Fructus, has been performed. However, previously reported methods are not considered accurate enough because only geniposide or gardenoside was chosen to be the marker component for the quality control of Gardeniae fructus. Thus, we developed the method using simultaneous determination of four components including geniposide, gardenoside, geniposic acid and chlorogenic acid. Against this backdrop, this study aims to propose a new calculation for gardenoside and geniposide concentrations by analyzing their concentrations in Gardeniae fructus.