Simultaneous quantification of six major phenolic acids in the roots of Salvia miltiorrhiza and four related traditional Chinese medicinal preparations by HPLC-DAD method

A high-performance liquid chromatographic method was applied to the determination of danshensu, protocatechuic aldehyde, rosmarinic acid, lithospermic acid, salvianolic acid B and salvianolic acid A in the roots of Salvia miltiorrhiza and four related traditional Chinese medicinal preparations. The six phenolic acids were simultaneously analyzed with a Zorbax Extend C18 column by gradient elution using 0.026% (v/v) phosphoric acid and acetonitrile as the mobile phase. The flow rate was 1 ml min(-1), and detection wavelength was set at 288 nm. The recovery of the method was in the range of 95.1-104.8%, and all the compounds showed good linearity (r > 0.9997) in a relatively wide concentration range. This assay was successfully applied to the determination of six major phenolic acids in 32 samples. The results indicated that the developed HPLC assay could be readily utilized as a quality control method for S. miltiorrhiza and its related traditional Chinese medicinal preparations.     

A gradient HPLC method for the quality control of chlorogenic acid, linarin and luteolin in Flos Chrysanthemi Indici suppository

The Flos Chrysanthemi Indici suppository, a famous traditional Chinese medicine, is marketed for the treatment of prostatitis and chronic pelvic inflammation. A simple, relatively rapid and accurate high-performance liquid chromatographic (HPLC) method was applied to the simultaneous determination of chlorogenic acid, linarin and luteolin in Flos Chrysanthemi Indici suppository. The good separation was achieved on a Hypersil ODS column by a gradient elution using the mixture of acetonitrile and aqueous 1.0% acetic acid as mobile phase within 23 min. The method was validated for three active phenolic compounds with the relative standard deviations (R.S.D.) of intra- and inter-day precision below 3.0%, and the detection limits (S/N=3) of chlorogenic acid, linarin and luteolin were 0.32, 0.08 and 0.05 microg ml(-1), respectively. This assay was successfully applied to the determination of three active phenolic compounds in Flos Chrysanthemi Indici suppository samples with the quantitative recoveries in the range of 94.7-101.8%. The results indicate that the developed HPLC method can be readily utilized as a quality control method for Flos Chrysanthemi Indici suppository and its related traditional Chinese medicinal preparations.     

Determination of hydrochlorothiazide, triamterene and propranolol hydrochloride by the spectrophotometric method and high-performance liquid chromatography (HPLC)

Spectrophotometric and chromatographic (HPLC) methods for determination of hydrochlorothiazide, triamterene and propranolol hydrochloride were elaborated. Both methods were appropriate for the determination of three compounds in pharmaceutical preparations containing their mixtures. Both the elaborated methods for the determination of the studied compounds give comparable results and can successfully be applied to the assay in their mixtures occurring in the composition of pharmaceutical preparations.     

清喉咽合剂中黄芩苷不同定量方法对比研究

目的：对比不同分析方法对清喉咽合剂中黄芩苷含量测定的影响。方法：采用高效液相色谱法和正交函数光谱法对清喉咽合剂中黄芩苷进行含量测定。结果：正交函数光谱法黄芩苷在0．045—0．225mg·ml-1范围内正交系数与浓度C之间呈现较好的线性关系,回归方程｜P2｜=0．0917C-0．0059（r=0．9999）;正交函数光谱法与HPLC法测定结果比较,差异无统计学意义（P〉0．05）。结论：正交函数光谱法简便、快速、准确,检测成本低,可以对中药制剂中主要活性成分进行快速、准确的定量检测。     

Simultaneous determination of prostaglandins (PG) E2, A2 and B2 and stability studies of PGE2 in pharmaceutical preparations by ion-pair reversed phase HPLC

In previous reports a direct thin-layer chromatographic method (TLC) for the determination of prostaglandins (PG) E2, A2, B2 and F2 alpha and a High-Performance Liquid Chromatographic method (HPLC) for the determination of PGE2-, PGA2- and PGB2- descendants and for stability studies of PGE2-descendant in pharmaceutical preparations were described In this paper the described HPLC method and a newly developed technique based on ion-pair HPLC are given for the simultaneous determination of PGE2, PGA2 and PGB2 and for the stability studies of PGE2 in pharmaceutical preparations. The extraction of PG's from pharmaceutical preparations is performed in a fully automated, electronically controlled extraction apparatus within 3 minutes. Ion-pair reversed phase HPLC is performed on a column of LiChrosorb RP18 using either methanol-water-octan-1-sulfonic acid sodium salt (55 ml + 45 ml + 65 mg) or methanol-water-tetrabutylammoniumperchlorate (360 ml + 290 ml + 1.0 g) as eluent. HPLC separation can also be performed on a column of mu-Bondapack C18 using methanol-n-butanol-glacial acetic acid-water (350 ml + 45 ml + 5 ml + 400 ml) as solvent. The stability of PGE2 is investigated in pure substance, in ethanolic-aqueous solution, in absolute ethanolic solution and in freeze-dried ampoules. The examined preparations are stored at temperatures between 4 and 40 degrees C and are investigated periodically. The stability studies of PGE2 indicate that PGA2 and PGB2 are formed as degradation products of PGE2. The prediction of the stability studies of PGE2 indicate that this active drug is unstable in pure substance as well as in pharmaceutical preparations.(ABSTRACT TRUNCATED AT 250 WORDS)     

Liquid chromatographic determination of folic acid in multivitamin preparations

A reversed-phase high-performance liquid chromatographic method is described for a stability-indicating assay of folic acid in multivitamin preparations. This method shows excellent recovery and precision characteristics, allows the determination of folic acid to levels of 0.1 microgram/mL, is simple to execute, and is suitable for high volume routine work. A good correlation was demonstrated between the HPLC method and the currently used bioassay.     

Combinative method using HPLC quantitative and qualitative analyses for quality consistency assessment of a herbal medicinal preparation

A selective and efficient quality consistency assessment system was developed for monitoring the manufacturing processes of a Chinese herbal preparation, qingfu guanjieshu (QFGJS) capsule, and for assessing its stability over time. This system is based on quantitative determination of four marker compounds, i.e., sinomenine, paeoniflorin, paeonol, and curcumin, and on qualitative fingerprinting analysis of QFGJS using high-performance liquid chromatography-photodiode array detection (HPLC-DAD) method. The separation was performed on a Phenomenex ODS column by gradient elution with acetonitrile and aqueous phase (containing 0.1% phosphoric acid, adjusted with triethylamine to pH 3.5+/-0.2) at a flow-rate of 1.0 ml/min. In fingerprinting analysis, the chemical characteristics of four herbs present in QFGJS (excluding radix Aconiti Lateralis Preparata) were present in the HPLC chromatographic file. In addition, quantitative determination of hypaconitine was carried out with our published HPLC method as a supplement for quality control of the radix Aconiti Lateralis Preparata in QFGJS. The results showed that the contents of these five marker compounds and HPLC fingerprint profiles of three batches of QFGJS products collected at 3 months after production in the stability testing were relatively consistent. This well-developed method could be used for quality assessment of the complex preparations of herbal medicine.     

Simultaneous determination of nine saponins from Panax notoginseng using HPLC and pressurized liquid extraction

A HPLC and pressurized liquid extraction (PLE) method was developed for simultaneous determination of nine saponins, including notoginsenoside R1, ginsenoside Rg1, Re, Rf, Rb1, Rc, Rb2, Rb3 and Rd in Panax notoginseng. The analysis was performed on C18 column with water-acetonitrile gradient elution and the investigated saponins were authenticated by comparing retention time and mass spectra with their reference compounds. Several methods including PLE, ultrasonication, soxhlet extraction and immersion were used for sample preparation and their extraction efficiency was compared. The results showed that PLE has the highest extraction efficiency and repeatability, which would be valuable on standardization of sample preparation for quality control of Chinese medicines. The developed HPLC and PLE is an effective approach for simultaneously quantitative determination of sapoinins in P. notoginseng, which could be used for quality control of P. notoginseng and its preparations.     

Simultaneous determination of vitamins A, D3 and E in multiple pharmaceutical preparations by HPLC method

This study makes possible the use of reversed phase HPLC with detection at 265 nm for the simultaneous quantitative determination of vitamin A, D3 and E in multiple pharmaceutical preparations. We have also proposed a very simple method of isolation of these vitamins from multivitamin preparations. On the basis of statistical analysis of the data, we can note that conditions for HPLC method used in our work gave us precise and accurate results.     

Determination of some beta-blockers as dabsyl derivatives by HPLC

A HPLC method has been developed that permits the sensitive determination of beta adrenergic blocking drugs, including acebutolol, metoprolol, oxprenolol, pindolol, and propranolol. These compounds were converted to their chromophoric dabsyl derivatives and were separated by a reversed phase chromatographic column (mu-Bondapak C18) with methanol-water (75:25) as isocratic mobile phase. The derivatives were detected by a variable wavelength detector operating at 430 nm. The method was applied to commercial pharmaceutical preparations and the results were statistically compared with those obtained by official methods using t- and F-tests.     

A reversed phase high performance liquid chromatography method for the analysis of boswellic acids in Boswellia serrata.

An HPLC method for the separation of boswellic acids, the active constituents in Boswellia serrata resin has been developed. The first accurate determination of 6 individual acids was possible in the resin as well as in multi-component preparations. By using an acidic mobile phase, raised temperature and a 4 microm Synergi MAX-RP 80 A column the acids could be detected at levels as low as 0.9 microg/ml. The study of market products revealed significant variations in the content of these pharmacologically active compounds in commercial samples.     

大青叶和板蓝根药材及其制剂质量控制的研究

首次提出以2,4(1H,3H)喹唑二酮[2,4(1H,3H)quinazolinedione]作为马蓝、蓼蓝药材及其制剂的质量控制指标。此成分系最近发现的,含量稳定且有代表性,尤其适用于评价此类中药制剂的真伪优劣,为当前难以解决的感冒退热冲剂和板蓝根冲剂的质量监控提供了可靠的方法。特别要指出的是本文是在高效液相色谱法中采用变换检测波长和梯度洗脱的方法,一次进样即可完成三种化学性质不同组分的含量分析,缩短了分析时间,提高了分析效率。     

Rapid and sensitive HPLC method for the simultaneous determination of dorzolamide hydrochloride and timolol maleate in eye drops with diode-array and UV detection

A rapid and sensitive HPLC method has been developed for the simultaneous determination of dorzolamide hydrochloride and timolol maleate. The drugs were monitored with a diode-array detector at two fixed wavelengths (lambda = 250.0 nm for dorzolamide hydrochloride and 300.0 nm for timolol maleate). Liquid chromatography was performed on a RP-YMC pack ODS A-132 C18 (5 microm, 15 cm x 6.0 mm) column and the mobile phase consisted of an acetonitrile: phosphate buffer (pH 2.5): methanol (5:85:10 v/v/v) mix and a flow rate of 1.2 ml x min(-1). The linearity of the method ranged between 4.0-45.0 microg x ml(-1) for dorzolamide hydrochloride and and 2.0-20.6 microg x ml(-1) for timolol maleate in binary mixture. The procedure was successfully applied to the determination of these compounds in pharmaceutical preparations and gave a high recovery, good accuracy and precision without any interference by the excipients.     

Application of orthogonal functions to the determination of prednisolone and hydrocortisone in some pharmaceutical preparations

Glenn's method of orthogonal functions has been successfully applied to the direct spectrophotometric determination of the title compounds in presence of phenylephrine and/or neomycin sulphate without preliminary separation. The proposed methods when applied to the analysis of market preparations are in good agreement with those of the triphenyltetrazolium colour reaction recommended as the official method.     

HPLC法测定双黄连制剂中连翘苷的含量

目的：在双黄连类制剂的质量标准中建立连翘苷的含量测定项。方法：ＨＰＬＣ法测定双黄连制剂中连翘苷的含量。使用ＯＤＳ柱,以乙腈－水（２５：７５）为流动相,检测波长为２７７ｎｍ。结果：此方法线性关系良好,平均加样回收率为９９．１％,ＲＳＤ＝０．８２％。结论：该方法精度高,分离度、重复性良好,结果准确可靠,可用于双黄连类制剂的质量控制。     

中药保健品中他达拉非的检测

目的:建立测定中药保健品中掺入化学药他达拉非的方法。方法:采用高效液相色谱-质谱联用法对两种样品进行了色谱分离及质谱鉴定。结果:两样品中检测物质的色谱行为,与质谱行为,均与他达拉非对照药品一致,表明两种胶囊样品中均含有他达拉非。结论:方法简便,快速,专属性好,适用于中药保健品中他达拉非的检测。     

HPLC法测定卡莫司汀注射液的含量

目的建立HPLC法测定卡莫司汀注射液的含量。方法采用HPLC法,C18色谱柱（150mm×4．6mm,5μm）,流动相为乙腈．水（40：60）,检测波长为205nm,流速为1.0ml·min。结果卡莫司汀在4．697～46．97mg·L^-1之间线性良好（r=0．9999）,精密度和重现性都较好。结论方法准确,专属性强,适用于卡莫司汀注射液中卡莫司汀的含量。     

中药制剂及保健品中添加的10种抗高血压药物监测

目的建立抗高血压药物盐酸可乐定、氢氯噻嗪、酒石酸美托洛尔、盐酸哌唑嗪、盐酸普萘洛尔、苯磺酸氨氯地平、利血平、硝苯地平、尼群地平、尼莫地平10种化合物的HPLC快速检测方法。方法采用GRACE Prevail C18色谱柱;梯度洗脱方式;利用相对容量因子和紫外光谱相似度双指标进行定性;相对容量因子法进行定量分析。结果建立了同时测定10种抗高血压药物的HPLC方法;采用双指标进行定性,增加了HPLC定性的准确性;相对校正因子的含量测定法,有效减少对照品的使用,加快HPLC的分析速度。结论本文建立了双指标定性、相对校正因子测定含量的HPLC方法,可以同时测定10种抗高血压药物,适用于中药制剂及保健品非法添加的快速监测。     

氨酚曲马多片的有关物质方法学研究

目的：建立HPLC法检查氨酚曲马多片的有关物质的方法。方法：采用苯基键合硅胶色谱柱（4.6mm×25cm×5μm）,以四氢呋喃：三乙胺：水：三氟乙酸=8：0.1：92：0.1（最终混合溶液的pH值范围应为2.2-2.4）为流动相,检测波长为216nm,柱温20℃。结果：方法的专属性及耐用性良好;在盐酸曲马多进样量为5.151ng～41.208ng范围内,进样浓度与色谱峰面积线性关系良好。结论：本方法简便、快速、灵敏,可有效检测氨酚曲马多片中的有关物质。     

头孢呋辛酯胶囊的有关物质方法学研究

目的：建立HPLC法检查头孢呋辛酯胶囊有关物质的方法。方法：采用C18（4.6mm×250mm,5μm）色谱柱,以0.2mol/L磷酸二氢铵溶液-甲醇（62：38）为流动相,检测波长为278nm。结果：方法的专属性及耐用性良好;在头孢呋辛浓度为0.7545～15.09μg/ml范围内,进样浓度与色谱峰面积线性关系良好。结论：本方法简便、快速、灵敏,可有效检测头孢呋辛酯胶囊中的有关物质。