Antimicrobial,antioxidant and anticancer activities of Laurencia catarinensis,Laurencia majuscula and Padina pavonica extracts

The antimicrobial, antioxidant, and anticancer activities of ethanolic extract of Laurencia catarinensis, L. majuscula and Padina pavonica were determined. The highest antibacterial activity; 23.40?±?0.58?mm (00.98?µg/ml) and 22.60?±?2.10?mm (03.90?µg/ml) were obtained against Klebsiella pneumonia by Laurencia catarinensis and Padina pavonica, respectively. However, Padina pavonica showed excellent antibacterial activity against Bacillus subtilis (21.7?±?1.5?mm; 1.95?µg/ml), Staphylococcus aureus (21.7?±?0.58?mm; 1.95?µg/ml), Streptococcus pyogenes (20.7?±?1.2?mm; 1.95?µg/ml) and Acinetobacter baumannii (20.1?±?1.2?mm; 3.9?µg/ml). Moreover, the highest antifungal activity; 24.7?±?2.0?mm (0.98?µg/ml), 23.7?±?1.5?mm (0.98?µg/ml), 23.6?±?1.5?mm (0.98?µg/ml) was obtained by Padina pavonica against Candida tropicalis, C. albicans and Aspergillus fumigatus, respectively. The algal extracts showed DPPH radical scavenging activity in a concentration–dependent manner with maximum scavenging activity (77.6%, IC₅₀?=?5.59?µg/ml and 77.07%, IC₅₀?=?14.3?µg/ml) was provided by Padina pavonica and Laurenica majuscula, respectively. The in vitro antitumor activity revealed that the IC₅₀ values of Padina pavonica were 58.9, 115.0, 54.5, 59.0, 101.0, 101.0, and 97.6?µg/ml; Laurencia catarinensis were 55.2, 96.8, 104.0, 78.7, 117.0, 217.0, 169.0?µg/ml; and Laurencia. majuscula were 115.0, 221.0, 225.0, 200.0, 338.0, 242.0, and 189.0?µg/ml; respectively against A-549 (Lung carcinoma), Caco-2 (Intestinal carcinoma), HCT-116 (Colon carcinoma), Hela (Cervical carcinoma), HEp-2 (Larynx carcinoma), HepG-2 (Hepatocellular carcinoma), and MCF-7 (Breast carcinoma) cell lines.     

Stability study of a clonidine oral solution in a novel vehicle designed for pediatric patients

Abstract

Clonidine hydrochloride is administered to opioid-addicted mothers’ neonates to reduce neonatal abstinence syndrome. It is prescribed off-label to neonates at 0.5–1 µg/kg/6?h, alone or in combination. The commercially injectable form of clonidine—Catapressan^® 0.15?mg/mL—is being orally given after an appropriate dilution in water. However, this practice is not suitable for a perfectly safe and accurate administration. The objectives were to design a 10 µg/mL oral solution of clonidine hydrochloride in Inorpha^® and to study the stability of this solution by a validated stability-indicating liquid chromatography (LC) method. The chemical, physicochemical and microbiological stability of the compounded formulation stored at 5?±?3?°C and 25?±?2?°C was tested over 60 days. The LC method used is specific, linear, accurate and precise. Upon storage between 2 and 8?°C according to classical and ‘in use’ schedules, the concentrations of clonidine and potassium sorbate (preservative) were found to be between 90.0 and 110.0% of the initial concentration, the pH between 4.4 and 4.7 and no microbial growth was noted. The stability of clonidine hydrochloride oral solution in Inorpha^® sets the basis for individualized, easy and safe administration of clonidine in pediatric populations.     

反相高效液相色谱法同时测定氨溴特罗口服液中盐酸氨溴索和盐酸克伦特罗的含量

目的：建立同时测定氨溴特罗口服溶液中盐酸氨溴索和盐酸克伦特罗含量的方法。方法采用RP－HPLC法测定,Agilent C18（4．6mm ×250mm,5μm）色谱柱,流动相为乙腈－0．01mol? L －1磷酸二氢钾溶液（加入0．4％三乙胺,用磷酸调 pH至3．5）（23∶77）;流速：1．0mL? min －1,检测波长：244nm,柱温35℃;进样量：20μL。结果盐酸氨溴索和盐酸克伦特罗分离良好,盐酸氨溴索在0．28475～2．278mg? mL －1（r＝0．9999）盐酸克伦特罗在0．494～247μg? mL －1（ r＝1）范围内线性良好。结论该法操作简单,耗时较短,可以用于氨溴特罗口服溶液的定量分析。     

积分脉冲安培检测-高效阴离子交换色谱法测定盐酸氨基葡萄糖口腔崩解片含量

目的建立测定盐酸氨基葡萄糖口腔崩解片含量的方法。方法采用积分脉冲安培检测-高效阴离子交换色谱法测定盐酸氨基葡萄糖,优化了淋洗条件和积分脉冲安培检测条件。结果盐酸氨基葡萄糖的检测限为0.05 ng,线性范围为0.1~40μg/mL,盐酸氨基葡萄糖口腔崩解片的加样回收率为100.1%,RSD为1.17%(n=9)。结论此法可简单、快速、灵敏、准确地测定盐酸氨基葡萄糖口腔崩解片的含量。     

Antiviral activity of arbidol hydrochloride against herpes simplex virus I in vitro and in vivo

Herpes simplex virus type 1 (HSV-1) causes significant human diseases ranging from skin lesions to encephalitis, especially in neonates and immunocompromised hosts. The discovery of novel anti-HSV-1 drugs with low toxicity is required for public health. Arbidol hydrochloride (ARB) is an indole derivative molecule with broad-spectrum antiviral activity. In this study, the antiviral effects of ARB against HSV-1 infection were evaluated in vitro and in vivo. The results showed that ARB presents significant inhibitory effect on HSV-1 plaque formation and generation of progeny virus, with EC50 values (50% effective concentration) of 5.39?µg/mL (10.49?µM) and 2.26?µg/mL (4.40?µM), respectively. Moreover, time-of-addition and time-of-removal assays further suggested that ARB has viral inhibitory effects when added up to 12?h post-infection (p.i.), which could be further corroborated by determining the expression of viral immediate-early (ICP4, ICP22 and ICP27), early (ICP8 and UL42) and late (gB, gD, gH, VP1/2 and VP16) genes by real-time quantitative PCR as well as the expression of viral protein ICP4 and ICP8 at 6?h and 12?h p.i. Results of the in vivo study showed that ARB could reduce guinea pig skin lesions caused by HSV-1 infection. Conclusively, this report offers new perspectives in the search for therapeutic measures in the treatment of HSV-1 infection.     

Quantitative determination of flavonoids and cycloartanol glycosides from aerial parts of Sutherlandia frutescens (L.) R. BR. by using LC-UV/ELSD methods and confirmation by using LC–MS method

This paper describes the first analytical method for the determination of four flavonoids (sutherlandins A–D) and four cycloartanol glycosides (sutherlandiosides A–D) from the aerial parts of Sutherlandia frutescens (L.) R. Br. A separation by HPLC was achieved by using a reversed phase (RP-18) column, PDA with ELS detection, and a water/acetonitrile gradient as the mobile phase. The wavelength used for quantification of four flavonoids with the diode array detector was 260 nm. Owing to their low UV absorption, the cycloartanol glycosides were detected by evaporative light scattering. The method was validated for linearity, repeatability, limits of detection (LOD) and limits of quantification (LOQ). The limits of detection and limits of quantification of eight compounds were found to be in the range from 0.1 to 7.5 μg/mL and 0.5 to 25 μg/mL, respectively. The analysis of products showed considerable variation of 1.099–5.224 mg/average weight for the major compound, sutherlandioside B. The eight compounds in plant sample and products of S. frutescens were further confirmed by LC–ESI-TOF. This method involved the use of the [M+H]⁺ and [M+Na]⁺ ions in the positive ion mode with extractive ion monitoring (EIM).     

Development and validation of a new HPLC analytical method for the determination of diclofenac in tablets

A new selective and sensitive high-performance liquid chromatography (HPLC) method was developed for the quantification of diclofenac sodium (DS) in pharmaceutical dosage form using lidocaine as internal standard (IS). Chromatographic separation was achieved on a symmetry C18 column (4.6?mm?×?150?mm, 3?μm spherical particles) using 0.05?M orthophosporic (pH 2.0) 35% and acetonitrile as 65%, as the mobile phase at a flow rate of 2.0?mL/min and monitored at 210?nm. The run time was 2?min.The method was validated to fulfill International Conference on Harmonisation (ICH) requirements and this validation included specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision and robustness. The calibration curve was linear over the concentration range from 10 to 200?µg/ml, and lower limit of detection of 12.5?ng/ml. The accuracy and precision of the method were within the acceptable limit of ±20% at the lower limit of quantitation and ±15% at other concentrations. Diclofenac was unstable at room temperature it showed more than 25% loss after 24?h. While, DS is very stable at refrigerator 4?°C auto-sampler, freeze/thaw cycles and 30?days storage in a freezer at ?35?±?2?°C.All results were acceptable and this confirmed that the method is suitable for its intended use in routine quality control and assay of drugs.     

HPLC method development and validation for simultaneous detection of Arabinoside-C and doxorubicin

This paper describes a new validated high performance liquid chromatography (HPLC) method for the simultaneous determination of two anti-cancer drugs, Arabinoside-C (Ara-C) and doxorubicin hydrochloride (DOX). A simultaneous determination method saves cost and time as both drugs can be injected into a single HPLC system without the need to change or re-equilibrate with a new mobile phase. The objective of the study is to develop a simultaneous determination method of two anti-cancer drugs, Ara-C and DOX. The mobile phase consisted of a mixture (45:55) of acetonitrile:ammonium hydrogen phosphate aqueous solution (0.01?M) at pH 6.2 at a flow rate of 0.3?ml/min, with UV detection at 252?nm. Separation was achieved on a C-18 column (5 µm: 250?mm?×?4.6?mm) maintained at 30°C in a column oven. The method was linear between 325?ng/ml and 10 µg/ml for Ara-C and 625?ng/ml and 20 µg/ml for DOX. The limit of detection (LOD) was 20?ng/ml for Ara-C and 60?ng/ml for DOX. The developed HPLC method achieved good precision and accuracy as well as limit of quantitations. The developed and validated method is suitable to be used for routine analysis of Ara-C and DOX.     

An approach to enhanced stability: Formulation and characterization of Solanum lycopersicum derived lycopene based topical emulgel

Focus of the study was to design a novel and cost effective extraction technique for the lycopene from Lycopersicum esculentum L. fruit and to develop and characterize a stable emulgel formulation containing lycopene as an active ingredient as well as to design an analytical method to determine lycopene concentration in emulgel. Emulgel formulation was prepared and evaluated for its stability at different storage conditions, 8?°C, 25?°C, 40?°C, 40?°C?+?75% relative humidity (RH) and 50?°C, for 6?months. Results were statistically analyzed using two way ANOVA, Post-Hoc test and paired sample t-test at 5% significance level. Designed extraction technique presented comparable yield, 154.83?mg/Kg of tomato fruit, with all recoveries in the range of 145–156?mg/Kg of tomato. “P-values” calculated for different levels of stability parameters were <0.05, except at 50?°C and time points of 60th day and later. Analytical method designed was having linear range of lycopene 1–10?µg/mL with limit of detection 0.11?µg/mL and limit of quantification 0.34?µg/mL. All inter-day and intra-day recoveries were in the range of 94–105% while in all measurements RSD % was ≤5.36. It can be concluded that the extraction technique was cost effective with comparable results and analytical method was simple, robust, specific and sensitive enough to be used for lycopene concentration determination in emulgel formulation. Furthermore, designed formulation was stable even at high temperature of 40?°C and RH 75%.     

Capillary electrophoresis with electrochemiluminescence detection for simultaneous determination of proline and fleroxacin in human urine

The content of free proline (Pro) in body fluids is a biological parameter for patients with renal insufficiency and chronic uraemia. Fleroxacin (FLX) must be used cautiously because of adverse reactions. Its dosage must be adjusted according to the degree of renal insufficiency. In a clinical setting the simultaneous determination of Pro and FLX in body fluids is necessary for the rational utilization of FLX. A capillary electrophoresis (CE) method based on electrochemiluminescence (ECL) detection with Ru(bpy)₃²⁺ was developed for the simultaneous determination of Pro and FLX in human urine. Parameters related to separation and detection were investigated and optimized. The most favourable resolution and high sensitivity were obtained using a 15 mM phosphate buffer at pH 9.6 with the detection potential at 1.15 V. Under optimized conditions, the standard curves were linear in the range of 0.1–80 µg/mL for Pro and 0.1–100 µg/mL for FLX. Detection limits(3σ) of 0.3 ng/mL for FLX and 0.02 µg/mL for Pro were obtained. Relative standard derivations (RSDs) of the ECL intensity and the migration time were 3.2% and 0.9% for 4 µg/mL Pro and 3.7% and 1.2% for 4 µg/mL FLX, respectively. The recoveries were in the range of 94.8–99.6% for Pro with RSDs of 2.8%–3.6% and 94.7–97.8% for FLX with RSDs of 2.9%–3.7%. The proposed method was successfully applied to determine the amounts of Pro and FLX in human urine. Copyright © 2009 John Wiley & Sons, Ltd.     

Phytochemical standardization and biological activities of certain desert plants growing in Saudi Arabia

The phytochemical screening, antimicrobial and antitumor activities of Calendula tripterocarpa, Centarea sinaica, Centaurea pseudosinaica, Koelpinia linearis, Plectranthus arabicus, Plectranthus asirensis and Tripleurospermum auriculatum determined. The best antibacterial activity; 41.8?±?0.23?mm, 39.7?±?0.25?mm, 35.8?±?0.58?mm, 34.7?±?0.51?mm and 32.7?±?0.25?mm was obtained by Plectranthus arabicus against Klebsiella pneumonia, Tripleurospermum auriculatum against Bacillus subtilis, Centaurea pseudosinaica against Bacillus subtilis, Centaurea pseudosinaica against Stroptococcus pyogenes and Plectranthus arabicus against Staphylococcus epidermidis, respectively. While the highest antifungal activity; 35.9?±?1.15?mm, 34.6?±?0.34, 30.6?±?0.26?mm and 29.9?±?0.63?mm was obtained by Tripleurospermum auriculatum against Geotricum candidum, Candida albicans, C. tropicalis and Aspergillus fumigatus, respectively. The antitumor activity (IC₅₀) obtained by Centarea sinaica; 3.1?±?6.9?µg/ml, 14.3?±?3.1?µg/ml and 22.7?±?4.1?µg/ml was better than activity of vinblastine sulphate; 5.9?±?0.4?µg/ml, 59.7?±?2.1?µg/ml and 30.3?±?1.4?µg/ml against breast carcinoma (MCF-7), cervical carcinoma (Hela) and colorectal carcinoma (CACO), respectively. Plectranthus arabicus alcoholic extract showed higher antitumor activity; 15.3?±?5.3?µg/ml, 28.6?±?3.6?µg/ml and 24.3?±?4.1?µg/ml than vinblastine; 21.2?±?0.9?µg/ml, 59.7?±?2.1?µg/ml and 30.3?±?1.4?µg/ml against prostate carcinoma (Pc3), cervical carcinoma (Hela) and colorectal carcinoma (CACO), respectively. Also, the antitumor activity of Plectranthus asirensis against cervical carcinoma (Hela) (37.1?±?2.6?µg/ml) was potent than vinblastine sulphate (59.7?±?2.1?µg/ml). The obtained results of LD₅₀ and sub-chronic toxicity revealed that the plants have no toxicity.     

Development and validation of an ultra performance liquid chromatography method for venlafaxine hydrochloride in bulk and capsule dosage form

A simple, specific, accurate, and precise ultra performance liquid chromatographic method was developed and validated for the estimation of venlafaxine hydrochloride in tablet dosage forms. A acquity TM BEH column having C18, 100×2.1 mm i.d. in isocratic mode, with mobile phase containing dipotassium hydrogen phosphate: Acetonitrile (30:70 v/v; pH 7.00 with dilute o-phosphoric acid) was used. The flow rate was 0.75 ml/min and effluents were monitored at 227 nm. The retention time of venlafaxine hydrochloride was 0.548 min. The method was validated for specificity, linearity, accuracy, precision, limit of quantification, limit of detection, robustness and solution stability. Limit of detection and limit of quantification for estimation of venlafaxine hydrochloride were found to be 6.11 μg/ml and 20.33 μg/ml, respectively. Recoveries of venlafaxine hydrochloride in tablet formulations were found to be in the range of 99.3-99.5%. Proposed method was successfully applied for the quantitative determination of venlafaxine hydrochloride in tablet dosage forms.     

Simultaneous determination of synephrine,arecoline, and norisoboldine in Chinese patent medicine Si-Mo-Tang oral liquid preparation by strong cation exchange high performance liquid chromatography

Context: Chinese patent medicine Si-Mo-Tang oral liquid preparation (SMT) is composed of Aucklandia luppa Decne (Compositae), Citrus aurantium Linn (Rutaceae), Lindera aggregata (Sims) Kosterm (Lauraceae), and Areca catechu Linn (Arecaceae). Studies of SMT have been impeded due to the lack of quality control methods.

Objective: This study aimed to simultaneously determine three alkaloids including synephrine, arecoline, and norisoboldine in SMT for the first time.

Materials and methods: A strong cation exchange (SCX) high performance liquid chromatography (HPLC) method was developed to simultaneously determine synephrine, arecoline, and norisoboldine in SMT, and was compared with ion-pairing chromatography using regular reversed-phase chromatography columns. System suitability parameters of synephrine, arecoline, and norisoboldine using the SCX chromatography column were investigated.

Results: Results demonstrated that good separations were achieved on an Agilent SCX (250?×?4.6?mm, 5 µm) column at 35°C. The mobile phase consisting of methanol-0.2% phosphoric acid was delivered at a constant flow of 1.0?mL min^?1 and the eluent was monitored at 215?nm. The HPLC method showed good linearity for the examined concentration ranges of 2.55–255.0, 1.30–208.0, and 2.06–201.6 µg mL^?1 for synephrine, arecoline, and norisoboldine, respectively. The limits of quantification (S/N?=?10) were 2.55, 1.30, and 2.06 µg mL^?1, the limits of detection (S/N?=?3) were 1.53, 0.78, and 1.21 µg mL^?1, and average recoveries were 98.99, 95.63 and 99.04%, respectively, for synephrine, arecoline, and norisoboldine.

Discussion and conclusion: This method has been successfully applied to determine synephrine, arecoline, and norisoboldine in Chinese patent medicine SMT.     

An ecofriendly green liquid chromatographic method for simultaneous determination of nicotinamide and clindamycin phosphate in pharmaceutical gel for acne treatment

A new green micellar liquid chromatographic method was developed and validated for the quantitative estimation of nicotinamide (NICO) and clindamycin phosphate (CLD) in bulk and pharmaceutical gel formulation. The analytes are well resolved in less than 6.0 minutes using micellar mobile phase consisting of 0.10M sodium dodecyl sulfate (SDS), 0.3% triethylamine, and 10% 2-propanol in 0.02M orthophosphoric acid at pH 3.0, running through an Eclipse XDB-C₈ column (150 mm × 4.6 mm, 5 μm particle size) with flow rate 1.0 mL/min. The effluent was monitored with diode array detection at 210 nm. The retention times of NICO and CLD were 3.8 minutes and 5.6 minutes, respectively. The method was validated according to the International Conference on Harmonisation (ICH) guidelines in terms of linearity, limit of detection, limit of quantification, accuracy, precision, robustness, and specificity to prove its reliability. Linear correlation was achieved by plotting the peak area of each drug against its concentration. It was found to be rectilinear in the ranges of 1.0–40.0 μg/mL and 0.5–15.0 μg/mL with limits of detection of 0.06 μg/mL and 0.03 μg/mL and limits of quantification of 0.19 μg/mL and 0.09 μg/mL for NICO and CLD, respectively. The method was successfully implemented for the simultaneous determination of the analytes in their bulk powder and combined gel formulation with high % recoveries. The ease of sample treatment facilitates and greatly expedites the treatment with reduced cost and improved accuracy of the procedure.     

UV–Vis spectroscopic quantification of residual acetone during the development of nanoparticulate drug delivery systems

Methods for nanoparticles preparation often employ organic solvents in order to solubilize the non-polar constituents of the final nanostructures. In the research process, nanoparticles are assayed as aqueous suspensions in several cases, so that an excessive residual concentration of the organic solvent needs to be avoided since may lead to undesired secondary effects during biological tests. Despite the importance, residual solvent concentration is rarely determined, making necessary the development of quantification methods suitable for this purpose. Acetone is frequently used in drug delivery systems preparation, being capable to exert significant toxicities both, in vitro and in vivo. Thus, a simple and inexpensive UV–Vis spectrophotometric method is proposed to directly determine acetone from nanoparticles suspensions employing its reaction with vanillin. Central composite designs were employed to correct and optimize the quantification method, which was then validated according to international guidelines. The optimized method resulted accurate, precise, and linear in the range of 10–50?µg/mL, with an R² of 0.998 and limits of detection and quantification of 2.6 and 7.8?µg/mL, respectively. The effect of several surfactants employed during nanoparticles preparation was not detrimental to the method. The proposed procedure can be successfully applied to directly quantify acetone from nanoparticles suspensions.     

Optimization and validation of RP-HPLC method for simultaneous estimation of palbociclib and letrozole

A simple, rapid, and robust RP-HPLC method have been developed and validated to measure palbociclib (PB) and letrozole (LT) at single wavelength (254?nm). A isocratic elution of samples performed on Intersil C₈ (4.6?mm?×?250?mm particle size 5?μm) column with mobile phase consisting 0.02 M sodium dihydrogen phosphate buffer (pH 5.5): acetonitrile: methanol (80:10:10 v/v/v) delivered at flow rate 1.0?mL?min^?1. A good linear response was achieved over the range of 5–50?μg?mL^?1. The LODs for PB and LT were found to be 0.098 and 0.0821 µg?mL^?1, while the LOQs for PB and LT were 0.381–0.315 µg?mL^?1, respectively. The method was quantitatively evaluated in terms of system suitability test, linearity, precision, accuracy (recovery) and robustness as per standard guidelines. The method is simple, convenient and suitable for the analysis of PB and LT in bulk drug.     

Inhibition of herpes simplex virus 1 (HSV-1) and poliovirus (PV-1) by bacteriocins from lactococcus lactis subsp. lactis and enterococcus durans strains isolated from goat milk

Bacteriocins have unusual inhibitory activity, including antiviral properties, and this can be exploited to give alternative applications. Semi–purified bacteriocins of six lactic acid bacteria (LAB) strains isolated from goat milk (two Lactococcus lactis: GLc03 and GLc05, and four Enterococcus durans: GEn09, GEn12, GEn14 and GEn17) were tested for cytotoxicity in Vero cells (50% Cytotoxicity Concentration: CC₅₀), and for their antiviral activities against herpes simplex virus 1 (HVS-1) and poliovirus (PV-1). Semi-purified bacteriocins presented low cytotoxicity, with CC₅₀ varying from 256.2?µg/mL (GLc05) to 1084.5?µg/mL (GEn14). CC₁₀ was determined for all isolates (GLc03: 36.9?µg/mL; GLc05: 51.2?µg/mL; GEn09: 88.1?µg/mL; GEn12: 99.9?µg/mL; GEn14: 275?µg/mL; and GEn17: 62.2?µg/mL) and considered for antiviral activity assays. Antiviral activity before virus adsorption was recorded against PV-1 for GLc05 (4.9%), GEn09 (3.4%), GEn12 (24.7%) and GEn17 (23.5%), and against HSV-1 for GEn12 (27.9%), GEn14 (58.7%) and GEn17 (39.2%). Antiviral activity after virus adsorption was identified against PV-1 for GLc05 (32.7%), GEn09 (91.0%), GEn12 (93.7%) and GEn17 (57.2%), and against HSV-1 for GEn17 (71.6%). The results obtained indicate the potential of some bacteriocins, particularly those produced by E. durans strains investigated in the present study, in viral inhibition and their application as new antiviral agents.     

Buprenorphine and norbuprenorphine concentrations in human breast milk samples determined by liquid chromatography-tandem mass spectrometry

Buprenorphine (BUP) is considered to be safe during pregnancy. However, the extent of BUP transfer into breast milk has not been investigated thoroughly. Because the drug concentration in the milk is 1 of the determinants in the assessment of the exposure risk, a rapid and sensitive LC-MS/MS method has been developed and evaluated to measure BUP and norbuprenorphine (norBUP) concentrations in milk. A solid-phase and 2 liquid-liquid extraction procedures have been compared. The lower limits of detection and quantification were 0.05 ng/mL and 0.18 ng/mL for BUP and 0.05 ng/mL and 0.20 ng/mL for norBUP, respectively, using a sample volume of 0.5 mL milk. BUP and norBUP concentrations determined from 10 random breast milk samples collected over 4 successive days from a lactating woman during buprenorphine maintenance therapy ranged from 1.0 to 14.7 and 0.6 to 6.3 ng/mL, respectively. Drug exposure of the infant may be considered to be low. Further investigations may seek to extend these preliminary findings to evaluate an infant's level of BUP exposure through breast milk.     

Development and validation of an HPLC-DAD method for bis(12)-hupyridone and its application to a pharmacokinetic study

A rapid and simple method of high performance liquid chromatography with UV detection for the quantification of bis(12)-hupyridone in rat blood has been developed and validated. Chromatographic separation was carried out in an Agilent Extend C₁₈ 5 μm column (length, 250 mm; inner diameter, 4.6 mm) using a mixture of water–acetonitrile–trifluoroacetic acid (81:19:0.04, v/v/v) as the mobile phase at a flow rate of 1 mL/min, with detection at 229 nm. The method used for the bis(12)-hupyridone quantification showed linearity for concentration range of 0.1–7.5 μg/mL with r² = 0.9991. The limit of detection and quantification of this method were 0.05 μg/mL and 0.1 μg/mL, respectively. The intra- and inter-day variations of the analysis were less than 4.22% with standard errors less than 13.3%. The developed method was successfully applied to the pharmacokinetic study of bis(12)-hupyridone after intravenous administration of 5 mg/kg and intraperitoneal administration of 10 and 20 mg/kg in rats.     

HPLC法测定通宣理肺颗粒中盐酸麻黄碱及盐酸伪麻黄碱的含量

目的：建立通宣理肺颗粒中盐酸麻黄碱及盐酸伪麻黄碱含量的高效液相色谱测定方法。方法：色谱柱为SymmetryC18（250mm×4．6mm,5μm）,流动相为甲醇-0．1％磷酸（含0．1％三乙胺）（7：93）,流速1．00mL／min,检测波长210nm,柱温30℃,选样量10μL。结果：盐酸麻黄碱在4．46～89．20μg／mL浓度范围内与峰面积线性关系良好,r=0．9995（n=6）,平均回收率为100.7％,RSD为1.6％（n=9）;盐酸伪麻黄碱在2．11-42．20μg／mL浓度范围内与峰面积线性关系良好,r=0．9999（n=6）,平均回收率为100．7％,RSD为1．5％（n=9）。结论：本测定方法简便,结果准确,灵敏度高,重复性好,可用于通宣理肺颗粒的质量控制。