| High performance liquid chromatography(HPLC)and high performance capillary electrophoresis(HPCE)are the most important separation techniques in liquid separation method.The principle,character,and key factors of HPLC and HPCE technologies were described.The history,current situation and future trends of HPLC and HPCE were reviewed in this thesis.HPLC has greatly evolved into a major analytical technique that is routinely employed for the rapid,reliable and highly sensitive determination of numerous compounds in pharmaceutical analysis and quality control of cosmetic products.While HPCE also plays an important role in determination of impurities of pharmaceutical analysis,in chiral separation,as well as in illegal adulteration in cosmetic products,due to its speed,efficiency,reproducibility, ultra-small sample volume and ease of clearing up the contaminants.This review covers around 269 references including all types of chromatographic and hyphenated techniques reported in the latest two years.The present research work describes the studies of high performance liquid chromatography with electrochemical detection in the quality control of impurities in pharmaceutical preparations,and different types of chromatographic and hyphenated techniques in the analysis of illegal adulteration in cosmetic products.The major content is described as follows:1.HPLC-electrochemical detection of methotrexate and related substances in Methotrexate InjectionAn HPLC-ECD method to separate and determine methotrexate and its related substances on an ODS column was established.A TSK-GEL@ODS-100SP column (150 mm×4.6 mm,5μm)was used as analytical column with a mobile phase consisted of acetonitrile-0.2mol·L-1phosphate buffer(pH6.0)(10:90).The flow rate was 1.0 mL·min-1,the column temperature was 35℃,and the working potential was 0.8V when using the glassy carbon disc electrode as the working electrode.The condition of electrochemical detection was studied and the difference between electrochemical detection and UV detection was compared.Methotrexate,aminopterin,and methopterin were separated.The linear range of methotrexate was 9.1-91μg·mL-1 (r=0.9999),the average recovery of the method was 100.4%(RSD=1.0%,n=9)。The detection limits of aminopterin,methopterin and methotrexate were 3.3,11 and 8.6ng,respectively.Compared with the UV detection method,the sensitivity of electrochemical dection is higher.It can be further employed in the detection of methotrexate in biosamples.2.Assay and determination of related impurities in Teniposide Injection by HPLC with electrochemical detectionA sensitive analytical method for related impurities of teniposide in Teniposide Injection based on high performance liquid chromatography(HPLC)separation and electrochemical detection(ECD)has been developed.A Phenyl-Hexyl and an ODS columns were used for the separation of teniposide,lignan P,alpha-thenylidene lignan P(ATLP),picrothenylidene lignan P(PTLP)and the excipients of the Injection.The condition of electrochemical detection was investigated and the difference between EC detection and UV detection was compared.Optimal separation and detection were obtained with a mobile phase of acetonitrile-water(38:62,v/v)on an ODS column and an EC detector(carbon disc electrode as the working electrode,the working potential was set at+0.7V vs.Ag/AgCl)within 10 minutes.Good linear relationship was established between peak current and concentration of analytes in the range of 0.1-9.6μg.mL-1for lignan P,0.1-9.0μg.mL-1for teniposide,0.1-5.8μg.mL-1for ATLP and 0.1-7.2μg.mL-1for PTLP.The limit of detection(LOD,S/N=3)was 0.2ng for lignan P,1.1ng for teniposide,1.0ng for ATLP and 0.7ng for PTLP.Compared with the UV detection method,the sensitivity of EC detection is largely enhanced.It can be employed efficiently in the quality control for impurities in Teniposide Injection with good selectivity and reproducibility.3.Determination of Entacapone and its related impurities by HPLC-ECDAn HPLC-electrochemical detection method was established for the determination of entacapone and its related impurities,z-isomer of entacapone and 3,4-dihydroxy-5-nitrobenzaldehyde.A phenyl column was used,using phosphate buffer(pH2.1) -methanol(54:46)as mobile phase.A glassy carbon disc electrode was used as the working electrode at the working potential of+0.65V.The calibration curve of entacapone,z-isomer and 3,4-dihydroxy-5-nitrobenzaldehyde were linear in the concentration range of 0.06-38.7μg.mL-1,0.06-42.5μg.mL-1and 0.06-27.5μg.mL-1. The detection limit was 0.05,0.06 and.03ng,respectively.The average recovery of entacapone was 99.9%with RSD 1.5%.4.Determination of six phenolic compounds in cosmetics by capillary electrophoresis with electrochemical detectionA method based on capillary electrophoresis with electrochemical(CE-ECD)to determine some phenolic compounds added in cosmetics was described.Effects of several factors,such as running buffer,potential applied to the working electrode, injection time and separation voltage were investigated to obtain the optimum conditions for separation and determination.With a 75 cm length of 25μm i.d. fused-silica capillary,well-defined separation of arbutin,phenol,resorcinol, hydroquinone,kojic acid and salicylic acid was achieved in the H3BO3-Na2B4O7(40 mmol.mL-1)running buffer with 10 mmol.mL-1SDS(pH 9.0).While operated in a wall-jet configuration,a 300μm carbon disc electrode used as the working electrode exhibits good response at+0.80V(vs.SCE)for these phenolic compounds.Good linear relationship was established between the peak current and the concentration of each analyte over 3 orders of magnitude with detection limit(S/N=3)ranging from 4.09×10-8g mL-1to 4.50×10-7g mL-1.The proposed method has been successfully applied for the determination of phenolic compounds in cosmetics with satisfactory results,provides a useful monitoring method for cosmetics safety.5.Simultaneous Determination of Antibiotics in Anti-acne Cosmetics by Rapid Liquid Chromatography with DADA suitable method that allows,for the first time,the simultaneous determination of nine antibiotics which may help the therapy of acne vulgaris by rapid high performance liquid chromatography with diode array detection(RPLC-DAD)in 7 minutes is presented in this work.A SB RP18(50 mm×4.6 mm;1.8μm particle size) column was used with the mobile phase consisted of a mixture of 0.1 mol.L-1 potassium dihydrogen phosphate(pH2.5)and acetonitrile at the gradient elution program.The correlation coefficients were all above 0.9999 in the linear range between 4-100μg mL-1,the average spiked recoveries(n=6)were 92.2%-103.2% with RSD ranging from 0.04%-4.5%depending on the target analytes.The method detection limits were in the range of 0.02-0.2μg mL-1in anti-acne cosmetics.The analysis of real cosmetic preparations demonstrated the fitness for the whole analytical procedure.The proposed method appeared therefore as a sound alternative for official testing method,which could overcome the general problems of time consuming,lack of the specificity and precision difficulty.6.Determination of Acrylamide residues in cosmetic products by liquid Chroma -tography with Tandem Mass SpectrometryA liquid chromatography coupled with electrospray ionization tandem mass spectrometry(LC-MS/MS)was established to the identification and quantification of acrylamide residues in cosmetic products.The method included defatting with petroleum ether,extraction with aqueous solution of 0.1%formic acid,further liquid-liquid extraction with petroleum ether.Acrylamide was detected with an Atlantis C18 column(2.1×150 mm,3μm)using 0.1%formic acid in water/0.1% formic acid in methanol(98:2)as mobile phase A,0.1%formic acid in methanol as mobile phase B in gradient elution mode.The analytical method in the present study was well verified and good results were obtained with respect to precision, repeatability and spiked recovery.
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