Abstract：
:This paper describes the development of simple and user-friendly HPLC methods that can quantitate the amount of small interfering RNA (siRNA) in lipid-based nanoparticle (LNP) formulations. The methods have been used as alternative chromatographic approaches to the size exclusion chromatography in order to perform "fit for purpose" analysis such as determining the amount of released siRNA from LNP formulations as a part of in-vitro release testing. Two HPLC conditions were optimized using reversed phase (a 250 × 4.6 mm Waters XSelect CSH column) and cation exchange columns (a 250 × 4.6 mm Zorbax SCX-300 column) maintained at 30 °C with a mobile phase of 0.1 M ammonium bicarbonate aqueous solution containing 20-30% acetonitrile. All the siRNA variants were excluded from pores in stationary phase and led to a single peak eluted earlier than the solvent front. The impact of chromatographic conditions and column configurations on method specificity, accuracy, and sensitivity have been investigated. Validation data for both methods in terms of precision, linearity, accuracy and sensitivity are also presented.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Huang Z,Fish WPdoi
10.1016/j.jpba.2019.04.026subject
Has Abstractpub_date
2019-08-05 00:00:00pages
253-258eissn
0731-7085issn
1873-264Xpii
S0731-7085(19)30344-9journal_volume
172pub_type
杂志文章abstract：:A sensitive method for the analysis of unconjugated morphine, codeine, normorphine and total morphine after hydrolysis of glucuronide conjugates is described. The method was applicable to 50-microliters volumes of plasma. The analytes were converted to heptafluorobutyryl (HFB) derivatives before analysis by gas chroma...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(94)00121-h
更新日期：1995-01-01 00:00:00
abstract：:The role of selenium as an antioxidant and anticancer agent is very well documented in the literature. Selenium compound showing the highest activity as a free radicals scavenger and as an anticancer agent should contain selenium at +4 oxidation level. The synthesis of selenitetriglycerides (named selol) was carried o...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00205-x
更新日期：2003-08-08 00:00:00
abstract：:A simple high-performance liquid chromatographic method was developed to study the pharmacokinetics of osthole in rat plasma. After addition of an internal standard (paeonol), plasma was deproteinized by acetonitrile for sample clean-up. The drugs were separated on a reversed-phase column and detected by UV absorption...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(95)01692-9
更新日期：1996-04-01 00:00:00
abstract：:Two analogs of sildenafil (compounds 1 and 2) were detected in three powder products acquired from online drug markets during an LC-UV-MS analysis of psychotropic drugs. Their structures were established by high-resolution mass spectrometry and NMR spectroscopy. Compound 1 was identified as 5-(5-(3,5-dimethylpiperazin...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.09.025
更新日期：2018-01-30 00:00:00
abstract：:Protein modification generally occurs by addition to the amino acid side-chains of protein at the post-translational stage, for example, by enzymatic or chemical reactions after polypeptide synthesis. Recently, the recombinant hirudin analog CX-397, a potent thrombin inhibitor, was found to contain methylated Ile resi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/s0731-7085(02)00703-3
更新日期：2003-04-01 00:00:00
abstract：:Sibutramine is one of the most occurring adulterants encountered in dietary supplements with slimming as indication. These adulterated dietary supplements often contain a herbal matrix. When customs intercept these kind of supplements it is almost impossible to discriminate between the legal products and the adulterat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.08.009
更新日期：2014-11-01 00:00:00
abstract：:In situ ATR-FTIR spectroscopy was used as a screening method to quantify the relative release of pamidronate (PAM) from films of polyelectrolyte (PEL) complex (PEC) particles. Stable colloid PEC particles consisting of poly(ethyleneimine) (PEI) and cellulose sulphate (CS) loaded with PAM were obtained by PEL complexat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.03.047
更新日期：2012-07-01 00:00:00
abstract：:Three methods are described for the simultaneous determination of mebeverine hydrochloride (MB) and sulpiride (SU) in combined pharmaceutical tablets. The first method depends on first-derivative ultraviolet spectrophotometry, with zero-crossing measurement method. The first derivative amplitudes at 214.2 and 221.6 nm...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(99)00176-4
更新日期：1999-11-01 00:00:00
abstract：:The stability indicating properties of the USP method for the assay of fentanyl in fentanyl citrate injection were evaluated [1] by analyzing fentanyl drug substance and product after acid, hydrogen peroxide, heat, and light treatment. N-phenyl-N-(4-piperidinyl)propionamide (PPA), which is a known degradation product/...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(99)00077-1
更新日期：1999-08-01 00:00:00
abstract：:Camazepam [3-(N,N-dimethyl)carbamoyloxy-7-chloro-1-methyl-1, 3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one, CMZ] possesses anxiolytic, anticonvulsant, muscle relaxant and hypnotic properties. CMZ is clinically used as a racemate. The enantioselective metabolism of racemic CMZ by rat liver microsomes was studied. Major...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(93)80103-8
更新日期：1993-11-01 00:00:00
abstract：:In this study, a selective sample pretreatment procedure combing surface molecularly imprinted polymers and microextraction in packed syringe (SMIPs-MEPS) was developed for the analysis of clenbuterol (CLB) from pork samples. SMIPs for CLB were synthesized on silica gel particles through a sol-gel process. A series of...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2013.12.022
更新日期：2014-03-01 00:00:00
abstract：:A PVC (polyvinychloride) ion selective electrode, employing benzyldimethyl-cetylammoniumbenzylpenicillin as sensor, was prepared, characterized and applied to the analysis of commercially available formulations containing benzylpenicillin and other antibiotics of the penicillin or cephalosporin group. The results are ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(88)80056-6
更新日期：1988-01-01 00:00:00
abstract：:Racecadotril, an enkephalinase inhibitor, was subjected to hydrolysis (acidic and alkaline), oxidation, photolysis and thermal stress, as per ICH specified conditions. The drug showed extensive degradation under acidic, basic hydrolysis and oxidative stress conditions whereas, it was stable under other stress conditio...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.05.008
更新日期：2016-09-05 00:00:00
abstract：:Due to severe chelating effect caused by N-hydroxylpyridone group of ciclopirox, there is no published direct HPLC or LC/MS/MS method for the determination of ciclopirox in any in vitro or in vivo matrix. Instead, the time-consuming pre-column derivatization methods have been adapted for indirect analysis of ciclopiro...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2009.08.019
更新日期：2010-01-05 00:00:00
abstract：:The objective of this paper is to evaluate the variations in the ability of Pistacia atlantica leaves to inhibit enzymes linked to type 2 diabetes (α-amylase and α-glucosidase) and to hypertension (angiotensin converting enzyme-I (ACE-I)), depending on harvesting month, gender and growing region, as well as to identif...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.11.049
更新日期：2018-02-05 00:00:00
abstract：:American ginseng (Panax quinquefolius) is originally grown in North America. Due to price difference and supply shortage, American ginseng recently has been cultivated in northern China. Further, in the market, some Asian ginsengs are labeled as American ginseng. In this study, forty-three American ginseng samples cul...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.06.031
更新日期：2014-10-01 00:00:00
abstract：:Indole-3-carbinol is a natural glucosinolate known for prevention of human breast, prostate and other types of cancer and it started to be used in commercial preparations, as food supplements. However no analytical method has been proposed for quality control of nutraceuticals with this substance yet. In this paper a ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.12.039
更新日期：2016-02-20 00:00:00
abstract：:A high-performance liquid chromatographic (HPLC) method is described for the assay of salmon calcitonin. The method uses a 5-microns octadecasilyl silica column (100 x 4.6 mm) at 50 degrees C and an initial mobile phase (flow rate 1 ml min-1) comprising 35% of B (1 M tetramethylammonium hydroxide-water-acetonitrile, 8...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(90)80118-9
更新日期：1990-01-01 00:00:00
abstract：:Recently it was found that normal adults excrete pipecolic acid primarily as the D-enantiomer even though it is present in the blood stream mainly as the L-enantiomer (i.e. > 98% L). This study of pipecolic acid stereochemistry was extended to subjects with peroxisomal deficiencies since they are known to have high le...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(93)80044-2
更新日期：1993-10-01 00:00:00
abstract：:A numerical method, based on the use of spectrophotometric data coupled to PLS-1 multivariate calibration, is reported for the simultaneous determination of furosemide and amiloride hydrochloride in synthetic samples and commercial tablets. The method was applied in the concentration ranges of 8.0-13.0 mg l(-1) for fu...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00432-0
更新日期：2001-10-01 00:00:00
abstract：:In this brief review a superficial introduction is given to the important area of biologically active carbohydrates. The complexity of carbohydrate chemistry is considered and the possible uses of carbohydrates as drugs and diagnostic agents are outlined. The analytical tools and methods that are especially useful for...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(86)80007-3
更新日期：1986-01-01 00:00:00
abstract：:Capillary electromigration techniques have become important tools for the analysis of pharmaceutical drugs. The present review updates on recent developments of the analysis of small molecule drugs, excipients and counter ions dating between January 2014 and May 2017. Capillary electrophoresis (CE) continues to be a v...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2017.06.063
更新日期：2018-01-05 00:00:00
abstract：:Capillary electrophoresis with conductivity detection is a selective and quantitative method for the analysis of counter cations, such as potassium, in pharmaceutical drug substances. It is also a sensitive and specific technique for screening and measuring inorganic impurities in drug substance samples. Both counter ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(99)00245-9
更新日期：2000-02-01 00:00:00
abstract：:A new method was developed for the simultaneous determination of nine major constituents in Dracocephalum rupestre, including 5,7-dihydroxychromone (1), eriodictyol-7-O-beta-d-glucoside (2), luteolin-7-O-beta-d-glucoside (3), naringenin-7-O-beta-d-glucoside (4), apigenin-7-O-beta-d-glucoside (5), eriodictyol (6), lute...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.09.013
更新日期：2008-12-15 00:00:00
abstract：:Trans-3,5,4'-trihydroxystilbene (trans-resveratrol, RES) exhibits very low bioavailability due to extensive conjugative metabolism. Whether RES metabolites exhibit pharmacologic activity is of great interest. The present study aimed at synthesis of monoconjugates of RES - the 3- and 4' monosulfates (R3S and R4'S), and...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.12.006
更新日期：2012-04-07 00:00:00
abstract：:Adulterations with synthetic drugs are common problems with herbal medicine and this can potentially cause serious adverse effects. It is therefore important to determine the presence of synthetic drugs in herbal medicine to ensure patients' safety. The objective of this study was to develop sensitive and specific met...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00637-4
更新日期：2003-02-26 00:00:00
abstract：:Potency is an important parameter for evaluation of quality of heparin active pharmaceutical ingredient (API). In this paper the feasibility to determine potency of heparin API with near infrared reflectance spectroscopy (NIRS) coupled with partial least squares (PLS) algorithm is attempted. PLS factors, correlation c...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2009.11.022
更新日期：2010-04-06 00:00:00
abstract：:Astemizole (AST), a second-generation antihistamine, is metabolized to desmethyl astemizole (DEA), and although it has been removed from the market for inducing QT interval prolongation, it has reemerged as a potential anticancer and antimalarial agent. This report describes a novel high-performance liquid chromatogra...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.04.036
更新日期：2015-10-10 00:00:00
abstract：:Four impurities in fluconazole API sample obtained from a recently proposed synthetic process were detected by HPLC. One of the impurities was unknown having not been reported previously. This less polar unknown impurity was isolated from the crude sample of fluconazole bulk drug using semi-preparative HPLC. Structure...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.06.029
更新日期：2007-11-05 00:00:00
abstract：:The simultaneous interaction of 15 steroidal drugs with tau-cyclodextrin (tauCD) and hydroxypropyl-beta-CD (HPbetaCD) was determined by charge transfer chromatography and the relative strength of interaction was calculated for each drug-tauCD-HPbetaCD ternary complex. The mixture of CDs interacted with each steroidal ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(99)00234-4
更新日期：2000-02-01 00:00:00
