Simultaneous quantification of Lamivudine and Zidovudine in tablets by HPTLC method was developed and validated.The chromatograms were developed using a mobile phase of toluene:ethyl acetate:methanol (4:4:2,v/v/v) on ...Simultaneous quantification of Lamivudine and Zidovudine in tablets by HPTLC method was developed and validated.The chromatograms were developed using a mobile phase of toluene:ethyl acetate:methanol (4:4:2,v/v/v) on pre-coated plate of silica gel GF aluminum TLC plate and quantified by densitometric absorbance mode at 276 nm.The R f values were 0.4170.03 and 0.6070.04 for Lamivudine and Zidovudine,respectively.The linearity of the method was found to be within the concentration range of 50 250 ng/spot for Lamivudine and for Zidovudine,it was 100 500 ng/spot.The lower limits of detection and quantification were 2.23 ng/spot and 7.90 ng/spot for Lamivudine and 2.90 ng/spot and 8.85 ng/spot for Zidovudine.The method was also validated for precision,specificity and recovery.This developed method was used to analyze fixed-dose tablets (Duovir,Cipla Ltd) samples of Lamivudine and Zidovudine.展开更多
Heteroclitin D （H.D） was successfully isolated from Kadsurae Caulis by using flash chromatography and recrystalllzed by methanol, 10.2 mg of H.D was obtained from 4.86 g of crude extract, and the purity determined b...Heteroclitin D （H.D） was successfully isolated from Kadsurae Caulis by using flash chromatography and recrystalllzed by methanol, 10.2 mg of H.D was obtained from 4.86 g of crude extract, and the purity determined by HPLC was 99.4%. The structure was identified by UV, IR, MS, and NMR analysis. The fast, simple and efficient method can be applied to the preparation of reference substance of H. D.展开更多
Given severe health-hazardous effects of aflatoxin B1(AFB1) widely occurring in cereal grains and animal feeds,it is highly urgent to develop analytical methods for its rapid screening.In this work,we proposed a simpl...Given severe health-hazardous effects of aflatoxin B1(AFB1) widely occurring in cereal grains and animal feeds,it is highly urgent to develop analytical methods for its rapid screening.In this work,we proposed a simple and high-throughput method for the determination of AFB1 in millet and buckwheat samples using high performance thin layer chromatography(HPTLC) linked to fluorescence densitometry.The first step was to optimize the solid-liquid extraction for the crude clean-up of the samples.The QuEChERS(Quick,Easy,Cheap,Effective,Robust and Safe) extraction strategy was used and different solvent systems for their extraction efficiency of AFB1 from the samples were evaluated.Then,trichloromethane:ethyl acetate(7:3,V/V) was used as the mobile phase to realize the separation of the targeted compound from background noises on silica gel plates.Quantification was readily performed with densitometry in fluorescence mode.In order to fix the optimal excitation wavelength,spectra scanning ranging 250-400 nm was carried out,revealing that 364 nm light gave the highest signal.With the optimized optical system,high sensitivity to AFB1 was achieved,with a limit of detection(LOD) at 3 μg/kg.Apart from that,good linearity(0.999) was obtained within the range of 1-80 ng/band of AFB 1.To assess the analysis accuracy,2 levels of AFB 1(50 and100 μg/kg) were spiked into real grain samples.The obtained results showed that the recovery rates were within the range of 81.6%-114.0%.The proof-of-concept results of this work evidenced that HPTLC is a promising analytical tool for the screening of mycotoxin in difficult samples.展开更多
文摘Simultaneous quantification of Lamivudine and Zidovudine in tablets by HPTLC method was developed and validated.The chromatograms were developed using a mobile phase of toluene:ethyl acetate:methanol (4:4:2,v/v/v) on pre-coated plate of silica gel GF aluminum TLC plate and quantified by densitometric absorbance mode at 276 nm.The R f values were 0.4170.03 and 0.6070.04 for Lamivudine and Zidovudine,respectively.The linearity of the method was found to be within the concentration range of 50 250 ng/spot for Lamivudine and for Zidovudine,it was 100 500 ng/spot.The lower limits of detection and quantification were 2.23 ng/spot and 7.90 ng/spot for Lamivudine and 2.90 ng/spot and 8.85 ng/spot for Zidovudine.The method was also validated for precision,specificity and recovery.This developed method was used to analyze fixed-dose tablets (Duovir,Cipla Ltd) samples of Lamivudine and Zidovudine.
基金supported by the International Scientific and Technological Cooperation Program of China(No:2009DFA31230)the Industry-University-Research Cooperation Program from Science and Technology Department of Qingyuang City(No:2012D021211001)
文摘Heteroclitin D （H.D） was successfully isolated from Kadsurae Caulis by using flash chromatography and recrystalllzed by methanol, 10.2 mg of H.D was obtained from 4.86 g of crude extract, and the purity determined by HPLC was 99.4%. The structure was identified by UV, IR, MS, and NMR analysis. The fast, simple and efficient method can be applied to the preparation of reference substance of H. D.
基金supported by National Key Research and Development Program of China (2021YFF0601902)Shanxi Scholarship Council of China (2021-068)+1 种基金Opening Project of Key Laboratory of Detection for Mycotoxins, Ministry of Agriculture and Rural Affairs China (SWDSJC2021001)Shanxi Agricultural University High-Level Talent Project (2021XG013)。
文摘Given severe health-hazardous effects of aflatoxin B1(AFB1) widely occurring in cereal grains and animal feeds,it is highly urgent to develop analytical methods for its rapid screening.In this work,we proposed a simple and high-throughput method for the determination of AFB1 in millet and buckwheat samples using high performance thin layer chromatography(HPTLC) linked to fluorescence densitometry.The first step was to optimize the solid-liquid extraction for the crude clean-up of the samples.The QuEChERS(Quick,Easy,Cheap,Effective,Robust and Safe) extraction strategy was used and different solvent systems for their extraction efficiency of AFB1 from the samples were evaluated.Then,trichloromethane:ethyl acetate(7:3,V/V) was used as the mobile phase to realize the separation of the targeted compound from background noises on silica gel plates.Quantification was readily performed with densitometry in fluorescence mode.In order to fix the optimal excitation wavelength,spectra scanning ranging 250-400 nm was carried out,revealing that 364 nm light gave the highest signal.With the optimized optical system,high sensitivity to AFB1 was achieved,with a limit of detection(LOD) at 3 μg/kg.Apart from that,good linearity(0.999) was obtained within the range of 1-80 ng/band of AFB 1.To assess the analysis accuracy,2 levels of AFB 1(50 and100 μg/kg) were spiked into real grain samples.The obtained results showed that the recovery rates were within the range of 81.6%-114.0%.The proof-of-concept results of this work evidenced that HPTLC is a promising analytical tool for the screening of mycotoxin in difficult samples.
文摘目的:建立测定庆大霉素组分及其相关物质的 HPTLC 法。方法:用高效薄层色谱法测定庆大霉素组分及其相关物质。CAMAG 全自动薄层色谱仪;薄层板采用 MEREK 高效硅胶 G 板,展开剂为氯仿-甲醇-25%氨水(5:7:6),测定波长为485nm。结果:庆大霉素在3.98～39.8μg·mL^(-1)。范围内各组分呈良好的线性关系(r>0.99);检测限为 ng 级。庆大霉素注射液中组分及其相关小组分之间分离度良好。结论:该方法简单、快速,灵敏度高,适用于庆大霉素组分中相关物质的分离测定。
