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Designing a bacterial cellulose‐based hydrogel incorporated with manganese sulfide and graphene oxide for green extraction of acrylamide in bread samples 设计一种含有硫化锰和氧化石墨烯的细菌纤维素基水凝胶,用于面包样品中丙烯酰胺的绿色提取
Q3 Chemistry Pub Date : 2023-10-20 DOI: 10.1002/sscp.202300169
Hassan Sereshti, Fatemeh Rezvani, Sara Soltani, Faezeh Karami, Hamid Rashidi Nodeh
Abstract A novel nanocomposite based on bacterial cellulose (BC) modified by manganese sulfide (MnS) decorated graphene oxide (GO) was prepared. The hydrogel was characterized by Fourier transform infrared, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, and adsorption/desorption techniques. The sorbent was employed for determining acrylamide in bread samples using micro‐solid‐phase extraction coupled with high‐performance liquid chromatography. The extraction efficiency of prepared sorbent was 1.4‐fold higher than that of BC. The important extraction factors including elution conditions (acetonitrile 300 μL, 5 min), sorbent composition and mass (50 mg), adsorption time (7 min), sample solution pH (8), and salt effect (3% w/v) were considered for optimization of the method. The analytical merit was validated by assessing the preconcentration factor (178–225), limit of detection (1.56 μg/kg), limit of quantification (5.15 μg/kg), linearity (5.15–500 μg/kg), and determination coefficient (0.9845). The adsorption isotherms and kinetic studies demonstrated that the adsorption process followed the Langmuir model and pseudo‐second‐order kinetics. The relative recoveries and relative standard deviations were 84%–106% and 2.4%–9.2%, respectively. This paper is the first report on the fabrication and use of BC doped with MnS‐GO composite for extraction of acrylamide in typical commercial bread samples.
摘要制备了一种以硫化锰修饰氧化石墨烯(GO)修饰细菌纤维素(BC)为基础的纳米复合材料。通过傅里叶变换红外、扫描电镜、能量色散X射线能谱和吸附/解吸技术对水凝胶进行了表征。采用微固相萃取-高效液相色谱法测定面包样品中的丙烯酰胺。所制备的吸附剂的萃取效率是BC的1.4倍。考察了洗脱条件(乙腈300 μL, 5 min)、吸附剂组成和质量(50 mg)、吸附时间(7 min)、样品溶液pH(8)、盐效应(3% w/v)等因素对提取方法的影响。通过预富集系数(178 ~ 225)、检出限(1.56 μg/kg)、定量限(5.15 μg/kg)、线性度(5.15 ~ 500 μg/kg)和测定系数(0.9845)验证了该方法的分析价值。吸附等温线和动力学研究表明,吸附过程符合Langmuir模型和准二级动力学。相对加样回收率为84% ~ 106%,相对标准偏差为2.4% ~ 9.2%。本文首次报道了BC掺杂MnS - GO复合材料用于提取典型商业面包样品中的丙烯酰胺。
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引用次数: 0
Detection of synthetic lipid‐lowering adulterants in herbal products using high‐performance thin‐layer chromatography 高效薄层色谱法检测中药产品中合成降脂掺假物
Q3 Chemistry Pub Date : 2023-10-20 DOI: 10.1002/sscp.202300165
Hardi Joshi, Payal Bahliwala, Jigna Vadalia, Udaykumar Vegad
Abstract Adulterating herbal medicine with undeclared synthetic drugs is a worldwide problem that seriously threatens human health. To detect such illicit and not labeled synthetic hypolipidemic substances in herbal medicines, an analytical method to simultaneously identify and quantify atorvastatin (ATV) calcium, simvastatin (SIM), gemfibrozil (GEM), fenofibrate (FEN) belonging to two different classes of drugs (statins and fibrates) was developed based on high‐performance thin‐layer chromatography. The method consisted of Silica Gel G60 F 254 precoated aluminum plate as stationary phase and toluene: ethyl acetate: formic acid (7:3:0.3, v/v/v) as optimized mobile phase. The densitometric evaluation wavelength was optimized at 254 nm. The Rf values of ATV, SIM, GEM, and FEN were 0.157, 0.268, 0.691, and 0.852, respectively. The linearity range is between 100–1500 ng/band for ATV and FEN and 200–3000 ng/band for SIM and GEM, respectively. The accuracy was found to be in the range of 97%–105%. The relative standard deviation of precision and robustness was found to be < 5%. However, the five screened market samples did not show the presence of adulteration of the above drugs. This method for the simultaneous determination of four drugs may be successfully employed to screen synthetic hypolipidemics as adulterants in herbal products and dietary supplements.
摘要以未经申报的合成药物掺假中药材是严重威胁人类健康的世界性问题。为了检测中草药中非法和未标记的合成降血脂物质,建立了一种基于高效薄层色谱法同时鉴定和定量阿托伐他汀(ATV)钙、辛伐他汀(SIM)、吉非纤维齐(GEM)、非诺贝特(FEN)两类药物(他汀类药物和贝特类药物)的分析方法。该方法以硅胶g60f254预涂铝板为固定相,甲苯:乙酸乙酯:甲酸(7:3:3 .3,v/v/v)为优化流动相。密度评价波长优选为254 nm。ATV、SIM、GEM、FEN的Rf值分别为0.157、0.268、0.691、0.852。ATV和FEN的线性范围分别为100-1500 ng/波段,SIM和GEM的线性范围为200-3000 ng/波段。准确度在97% ~ 105%之间。精密度和稳健性的相对标准偏差为<5%. 但经筛选的5个市场样本均未发现上述药品存在掺假现象。同时测定四种药物的方法可成功地用于筛选草药产品和膳食补充剂中作为掺假物的合成低脂药。
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引用次数: 0
Simultaneous estimation of propyphenazone, flurbiprofen, and their mutual prodrug by high‐performance liquid chromatography method 高效液相色谱法同时测定丙苯那酮、氟比洛芬及其相互前药的含量
Q3 Chemistry Pub Date : 2023-10-19 DOI: 10.1002/sscp.202300104
Zanza Patel, Falguni Tandel, Rati Kailash Prasad Tripathi
Abstract The current work comprises of development of a simple, rapid, and precise reverse phase‐high‐performance liquid chromatography method for simultaneous estimation of propyphenazone, flurbiprofen, and their mutual prodrug. Column C18 (Shimadzu Shim‐pack Gist, 250 × 4.6 mm, 5 μm) was employed as a stationary phase, and the ratio of acetonitrile:methanol:water (40:40:20 %v/v) was used as the mobile phase. The flow rate was held at 1 mL/min and detection was carried out at 245 nm using an ultraviolet detector. The retention time of propyphenazone, flurbiprofen, and their mutual prodrug was found to be 4.0, 2.5, and 10.0 min, respectively. The proposed method was validated according to the International Council on Harmonization Q2(R1) guideline in terms of accuracy, precision, linearity, limit of detection, limit of quantitation, and solution stability. Calibration plots were linear over the concentration ranges of 2–10 μg/mL (R 2 = 0.9998, R 2 = 0.9992 and R 2 = 0.9994 for propyphenazone, flurbiprofen, and their mutual prodrug, respectively). Results of mean percentage recoveries were in the range of 99.6%–100.1% for flurbiprofen, 99.3%–100.2% for propyphenazone, and 99.9%–100.7% for prodrug, respectively. The developed method can be used for the assay of mutual prodrug and drug release study of the developed mutual prodrug also routine quality control evaluation of mutual prodrug in bulk form.
摘要建立了一种简单、快速、精确的反相高效液相色谱法,用于同时测定丙苯那酮、氟比洛芬及其相互的前药。色谱柱C18 (Shimadzu Shim‐pack Gist, 250 × 4.6 mm, 5 μm)为固定相,乙腈:甲醇:水(40:40:20 %v/v)为流动相。流速为1 mL/min,紫外检测器检测波长为245 nm。丙基非那酮、氟比洛芬及其相互前药的保留时间分别为4.0、2.5和10.0 min。根据国际统一理事会Q2(R1)指南对该方法进行了准确度、精密度、线性度、检出限、定量限和溶液稳定性等方面的验证。在2 ~ 10 μg/mL的浓度范围内,丙苯那酮、氟比洛芬及其前药分别呈线性关系(r2 = 0.9998、r2 = 0.9992、r2 = 0.9994)。结果氟比洛芬的平均回收率为99.6% ~ 100.1%,丙苯那酮的平均回收率为99.3% ~ 100.2%,前药的平均回收率为99.9% ~ 100.7%。该方法可用于制剂的前药含量测定和释药研究,也可用于制剂的常规质量控制评价。
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引用次数: 0
Solid‐phase extraction of losartan and chlordiazepoxide from biological samples using sponge‐activated carbon 海绵活性炭固相萃取生物样品中的氯沙坦和氯二氮环氧化物
Q3 Chemistry Pub Date : 2023-10-10 DOI: 10.1002/sscp.202300096
Saeid Khodadoust, Ferdous Pirayesh, Fatemeh Zeraatpisheh
Abstract In this research, sponge‐activated carbon was applied as an effective adsorbent for simultaneous dispersive solid ultrasound‐assisted microextraction followed by high‐performance liquid chromatography for the preconcentration and determination of losartan (LOS) and chlordiazepoxide (CDP) drugs from urine and plasma samples. The synthesized adsorbent was characterized using scanning electron microscopy and Brunauer–Emmett–Teller techniques. To investigate the effects of different parameters, such as adsorbent dosage, pH, adsorption time, and volume of extraction solvent on the extraction process of LOS and CDP, a central composite design (CCD)‐based response surface methodology was applied. Using a CCD, the optimized factors achieved an adsorption time of 13 min, an adsorbent dosage of 14 mg, an extraction solvent (methanol) of 1.3 mL, and pH = 4.7 under the desirability function. Under the optimized conditions, the presented method showed a wide linear range of 0.005–10.0 μg/mL with a limit of detections of 0.0011 and 0.0018 μg/mL for LOS and CDP, respectively. Moreover, the applied method had relative standard deviations of 4.7% and 5.3% for LOS and CDP, respectively.
摘要:本研究采用海绵活性炭作为有效吸附剂,同时进行分散固体超声辅助微萃取-高效液相色谱法对尿液和血浆样品中的氯沙坦(LOS)和氯二氮环氧化物(CDP)进行预富集和测定。采用扫描电镜和brunauer - emmet - teller技术对合成的吸附剂进行了表征。为了考察吸附剂用量、pH值、吸附时间和萃取溶剂体积等参数对LOS和CDP提取过程的影响,采用基于中心复合设计(CCD)的响应面法。在理想函数条件下,优化因子的吸附时间为13 min,吸附剂用量为14 mg,萃取溶剂(甲醇)为1.3 mL, pH = 4.7。在优化条件下,该方法在0.005 ~ 10.0 μg/mL范围内呈较宽的线性关系,对LOS和CDP的检出限分别为0.0011和0.0018 μg/mL。应用的方法对LOS和CDP的相对标准偏差分别为4.7%和5.3%。
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引用次数: 0
A novel method for the extraction and characterization of metabolites from Basidiomycota: Pleurotus ostreatus (Jacq.) P. Kumm., 1871 as a case study 担子菌(Pleurotus ostreatus)代谢物的提取与鉴定新方法p . Kumm。1871年作为案例研究
Q3 Chemistry Pub Date : 2023-10-10 DOI: 10.1002/sscp.202300116
Mirko Benvenuti, Simone Di Piazza, Annalisa Salis, Grazia Cecchi, Mirca Zotti, Sonia Scarfì, Gianluca Damonte
Abstract In recent years, the interest in the exploitation of fungal metabolites has grown considerably, given their application in numerous sectors involving human health. However, their identification and characterization by conventional analytical approaches is generally limited to single families of molecules per method of analysis. This constitutes a limiting factor of primary importance in the study of both the metabolic pattern of a single fungal sample and the discovery of its possible applications. In this work, a reverse‐phase high‐performance liquid chromatography coupled with mass spectrometry method for the profile determination of primary and secondary metabolites produced by the oyster‐mushroom Pleurotus ostreatus (Jacq.) P. Kumm., 1871, has been developed. By using a concomitant extraction in three different polarity‐decreasing solvents, namely methanol, ethanol, and acetonitrile, this method allowed the simultaneous analysis of all extracted metabolites belonging to the widest possible range of chemical families, giving an advantage for both qualitative and quantitative determination of known and unknown compounds. The method appears to be valuable and robust for the study of complex matrices like raw fungi extract such as those of Pleurotus ostreatu s cultivated on different substrates and/or exposed to multiple stressors.
近年来,鉴于真菌代谢物在涉及人类健康的许多领域的应用,人们对真菌代谢物开发的兴趣大大增加。然而,通过传统的分析方法,它们的鉴定和表征通常仅限于单个分子家族的分析方法。这在研究单个真菌样本的代谢模式和发现其可能的应用中构成了一个重要的限制因素。本研究采用反相高效液相色谱联用质谱法测定了平菇平菇(Pleurotus ostreatus, Jacq.)产生的初级和次级代谢产物。p . Kumm。1871年,已被开发。通过在三种不同的极性降低溶剂(即甲醇、乙醇和乙腈)中同时提取,该方法可以同时分析所有提取的代谢物,这些代谢物属于最广泛的化学家族,为已知和未知化合物的定性和定量测定提供了优势。该方法对于复杂基质的研究是有价值的和可靠的,如在不同基质上培养和/或暴露于多种应激源的平菇(Pleurotus ostreatu)的原始真菌提取物。
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引用次数: 0
Simultaneous detection and analysis of 11 nootropic compounds in 54 samples via liquid chromatography‐electrospray ionization‐tandem mass spectrometry and quadrupole time‐of‐flight mass spectrometry 采用液相色谱-电喷雾电离-串联质谱法和四极杆飞行时间质谱法对54个样品中的11种促智化合物进行了同时检测和分析
Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.1002/sscp.202300127
Nam Sook Kim, Hwan Seong Choi, Hyunil Shin, Ji Hyun Lee, Hyungil Kim, Sooyeul Cho
Abstract Dietary supplements used for improving brain function and strengthening attention are increasingly popular. However, illegal dietary supplements containing unapproved drugs continue to be seized. Therefore, it is necessary to rapidly screen and identify adulterated compounds in dietary supplements for public safety. To develop the simultaneous analytical method, we selected 11 nootropic compounds and optimized the simultaneous liquid chromatography‐electrospray ionization‐tandem mass spectrometry and optimal conditions for liquid chromatography‐quadrupole time‐of‐flight mass spectrometry were proposed to determine the fragmentation patterns of each compound. The specificity, linearity, limit of detection, limit of quantification, method detection limit, method quantitation limit, precision, accuracy, matrix effect, and stability of this method were evaluated according to international validation guidelines. The validated methods were applied to 54 samples containing dietary supplements and seized samples. On screening 11 nootropic compounds were detected in four solid samples (tablet and powder). By comparing the product ion ratios with the standards and quantification, vinpocetine (6.52–34.2 mg/g) was found in three samples, and omberacetam (995.6 mg/g) in one sample. To re‐confirm the detected compounds, the fragmentation patterns were compared with those of the standards using liquid chromatography‐quadrupole time‐of‐flight mass spectrometry. The developed simultaneous analysis method can help maintain public health and safety.
用于改善大脑功能和增强注意力的膳食补充剂越来越受欢迎。然而,含有未经批准药物的非法膳食补充剂继续被查获。因此,为了公共安全,有必要快速筛选和鉴定膳食补充剂中的掺假化合物。为了建立同时分析方法,我们选择了11种益智药化合物,并对液相色谱-电喷雾电离-串联质谱法进行了优化,并提出了液相色谱-四极杆飞行时间质谱法的最佳条件,以确定每种化合物的破碎模式。根据国际验证指南对该方法的特异性、线性度、检出限、定量限、方法检出限、方法定量限、精密度、准确度、基质效应、稳定性进行评价。将验证的方法应用于54份含有膳食补充剂的样品和查获的样品。通过筛选,在4种固体样品(片剂和粉剂)中检出11种促智化合物。通过与标准品和定量品的离子比比较,3个样品中检出长春西汀(6.52 ~ 34.2 mg/g), 1个样品中检出昂贝西坦(995.6 mg/g)。为了重新确认检测到的化合物,使用液相色谱-四极杆飞行时间质谱法将碎片模式与标准品的碎片模式进行比较。所开发的同步分析方法有助于维护公共卫生和安全。
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引用次数: 0
Synthesis and application of dual‐layer metal‐organic framework as a fiber coating based on copper‐based metal‐organic framework @ zeolitic imidazolate framework‐8 for solid‐phase microextraction of some selected parabens and their quantification using high performance liquid chromatography 基于铜基金属-有机骨架@沸石咪唑酯骨架- 8的双层金属-有机骨架纤维涂层的合成和应用,用于固相微萃取某些对羟基苯甲酸酯及其高效液相色谱定量分析
Q3 Chemistry Pub Date : 2023-10-05 DOI: 10.1002/sscp.202300141
Abeer Fadhil Mohammed, Milad Ghani, Jahan Bakhsh Raoof
Abstract Herein, the zeolitic imidazolate framework‐8 template was accommodated onto the surface of a pencil graphite substrate through the electrodeposition system. Then, Zn in the zeolitic imidazolate framework‐8 was replaced with Cu atoms via the galvanic replacement procedure. The modified template was used for the synthesis of another metal‐organic framework (copper‐benzene di carboxylic acid) by a solvothermal method. The prepared fiber was characterized by field emission‐scanning electron microscopy, Fourier transform infrared spectroscopy, and X‐ray diffraction technique. Then, it was employed for direct immersion solid‐phase microextraction of methyl, ethyl, and butyl parabens. Various factors, such as the pH of the sample solution, stirring rate, desorption volume, the concentration of salt, extraction time, and desorption time, were selected and optimized. Under the optimized condition (extraction time = 30 min, desorption time = 2 min, desorption volume = 200 μL, salt concentration = 0% w/v, sample solution pH = 3.0, and stirring rate = 700 rpm), the linearity of the method was in the range of 1–200 μg/L ( r 2 > 0.9926). The limits of detection and quantification fall between 0.28–0.65 μg/L and 0.91–1.98 μg/L, respectively. The analysis of selected parabens in toothpaste and hand and face lotion, were also done using the suggested methodology.
本文通过电沉积系统将沸石咪唑酸盐框架- 8模板安置在铅笔石墨衬底表面。然后,通过电替换程序将沸石咪唑盐框架- 8中的Zn替换为Cu原子。采用溶剂热法制备了另一种金属-有机骨架(铜-苯二羧酸)。利用场发射扫描电子显微镜、傅里叶变换红外光谱和X射线衍射技术对所制备的纤维进行了表征。然后,采用直接浸渍固相微萃取法提取对羟基苯甲酸甲酯、乙酯和丁酯。对样品溶液的pH、搅拌速率、解吸体积、盐浓度、萃取时间、解吸时间等因素进行了筛选和优化。在最佳提取时间为30 min,解吸时间为2 min,解吸体积为200 μL,盐浓度为0% w/v,样品溶液pH = 3.0,搅拌速度为700 rpm的条件下,该方法的线性范围为1 ~ 200 μg/L (r 2 >0.9926)。检测限为0.28 ~ 0.65 μg/L,定量限为0.91 ~ 1.98 μg/L。采用建议的方法对牙膏、洗手液和洗面乳中所选的对羟基苯甲酸酯进行了分析。
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引用次数: 0
A systematic review on bisphenols – Sources, health impacts, and analytical determination of bisphenol A in aqueous samples 双酚的来源、对健康的影响和水样中双酚A的分析测定的系统综述
Q3 Chemistry Pub Date : 2023-09-29 DOI: 10.1002/sscp.202300072
Veena Vinod, Amritha P S, Harathi P B
Abstract Bisphenol A and its structural analogs are used by industrial processes for the manufacture of plastics, and medical and electronic devices. When these products are disposed of, they tend to leach out causing pollution and impacting human health. Thus, many studies are focused on detecting the presence of Bisphenols in environmental matrices, especially in water and food, as it is a major route of human exposure. Advancements have been made in the preparation and detection of samples using different analytical techniques. The most widely used techniques for bisphenol detection are liquid chromatography and gas chromatography coupled with mass spectroscopy. The progress made for ultra‐trace detection of Bisphenols via the development of efficient sample extraction techniques and the benefits of each technique are highlighted. The recent advances in detection techniques using colorimetric and Raman spectroscopy are reviewed with an emphasis on the use of portable onsite techniques compared to conventional labor‐intensive and time‐consuming techniques. An overview of all the approaches to determining Bisphenols in environmental and food samples is discussed in detail to provide insight into the progress made in this field.
摘要双酚A及其结构类似物在工业过程中用于制造塑料、医疗和电子设备。当这些产品被丢弃时,它们往往会浸出,造成污染并影响人类健康。因此,许多研究都集中在检测环境基质中双酚类物质的存在,特别是在水和食物中,因为它是人类暴露的主要途径。使用不同的分析技术在制备和检测样品方面取得了进展。双酚检测最广泛使用的技术是液相色谱和气相色谱联用质谱。通过开发高效的样品提取技术,双酚超痕量检测取得了进展,并强调了每种技术的优点。本文综述了比色法和拉曼光谱检测技术的最新进展,重点介绍了与传统的劳动密集型和耗时技术相比,便携式现场技术的使用。概述了所有的方法来确定双酚类物质在环境和食品样品进行了详细讨论,以提供深入了解在这一领域取得的进展。
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引用次数: 0
Rapid identification of chemical constituents of Chaihu‐jia‐Longgu‐Muli decoction based on ultra‐performance liquid chromatography‐quadrupole time‐of‐flight mass spectrometry coupled with the UNIFI platform 基于超高效液相色谱-四极杆飞行时间质谱联用UNIFI平台快速鉴定柴胡-佳-龙骨-木里汤的化学成分
Q3 Chemistry Pub Date : 2023-09-22 DOI: 10.1002/sscp.202300103
Tong Wu, Yin Liu, Hanshuo Dong, Chunling Ai, Li Sun
Abstract Chaihu‐jia Longgu‐Muli decoction (CLMD) is a traditional Chinese medicine formula, and it has been used for more than a thousand years to treat mental and nervous system diseases. However, the active constitutions of the CLMD are unclear. Accordingly, an integrated analysis based on the ultra‐performance liquid chromatography‐quadrupole time‐of‐flight mass spectrometry method combined with the UNIFI platform was used to clarify the chemical composition of the CLMD. As a result, 102 compounds including 38 saponins, 32 flavonoids, 12 polyphenols, nine anthraquinones, and 11 others were identified or tentatively presumed. Among them, 19 compounds were confirmed unambiguously with standards. Moreover, the characteristic fragmentations and fragmentation patterns of different compounds in CLMD were summarized, and each compound was classified as an individual herb. It was demonstrated that this method is rapid and accurate and could provide a strategy for the qualitative analysis of the chemical constituents of CLMD, and these results will provide experimental evidence for the subsequent studies on the pharmacodynamic material basis and quality control of CLMD.
柴胡加龙骨木里汤(CLMD)是一种传统的中药方剂,用于治疗精神和神经系统疾病已有一千多年的历史。然而,CLMD的现行构成尚不清楚。因此,基于超高效液相色谱-四极杆飞行时间质谱法结合UNIFI平台的综合分析被用于澄清CLMD的化学成分。结果鉴定出102种化合物,包括38种皂苷、32种黄酮类化合物、12种多酚、9种蒽醌和11种其他化合物。其中,有19个化合物与标准相符合。此外,还总结了CLMD中不同化合物的特征片段和片段模式,并将每种化合物归类为单个草药。结果表明,该方法快速准确,可为CLMD化学成分的定性分析提供策略,为后续CLMD的药效学、物质基础和质量控制研究提供实验依据。
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引用次数: 0
Separation and quantitation of valacyclovir enantiomers using stability‐indicating chiral liquid chromatography method with a chiral stationary phase of amylose tris‐(3,5‐dimethylphenylcarbamate) 以直链淀粉三(3,5 -二甲基苯基氨基甲酸酯)为手性固定相,稳定性指示手性液相色谱法分离和定量伐昔洛韦对映体
Q3 Chemistry Pub Date : 2023-09-21 DOI: 10.1002/sscp.202300145
Niroja Vadagam, Sharath Babu Haridasyam, Muvvala Venkatanarayana, Narasimha S. Lakka, Sanjeeva R. Chinnakadoori
Abstract The present research developed and validated a new stability‐indicating technique for the stereo‐selectively enantiomers of the antiviral nucleoside analog Valacyclovir hydrochloride (VAL). The chiral separation was performed using normal‐phase high‐performance liquid chromatography (HPLC) with a chiral stationary phase consisting of amylose tris(3‐chloro‐5‐methylphenylcarbamate) and a mobile phase of “ n ‐hexane, methanol, ethanol, and diethylamine”, flow rate of 0.60 mL/min, column temperature of 30°C, injection volume of 10‐μL, detection wavelength of 254‐nm, and run time of 25‐min. The enantiomers (S‐enantiomer, L‐isomer, R‐enantiomer, and D‐isomer) of Valacyclovir were separated with a resolution of 4.8 and no interference. The validation parameters verified for the proposed method, linearity in a range of 0.1002–24.3486 μg/mL (0.02–4.86%) with a regression coefficient of 0.999, and the accuracy was determined with excellent recoveries ranging from 94.38%–109.97%. The concentrations established for the detection limit and quantitation limit were 0.01% and 0.02%, respectively. The forced degradation experiments were used to assess the stability‐indicating qualities. D‐Valacyclovir impurity was successfully evaluated in release and stability samples of VAL in drug substance and tablet dosage forms using the proposed normal phase chiral HPLC approach.
摘要:本研究开发并验证了一种新的抗病毒核苷类似物盐酸伐昔洛韦(Valacyclovir hydrochloride, VAL)立体选择性对映体的稳定性指示技术。采用正相高效液相色谱法进行手性分离,手性固定相为直链淀粉三(3‐氯‐5‐甲基苯基氨基甲酸酯),流动相为正己烷-甲醇-乙醇-二乙胺,流速为0.60 mL/min,柱温为30℃,进样量为10 μL,检测波长为254 μ nm,运行时间为25 min。Valacyclovir的对映体(S -对映体、L -异构体、R -对映体和D -异构体)在4.8的分辨率下无干扰分离。结果表明,该方法的线性范围为0.1002 ~ 24.3486 μg/mL(0.02 ~ 4.86%),回归系数为0.999,准确度为94.38% ~ 109.97%。建立的检测限和定量限浓度分别为0.01%和0.02%。采用强制降解实验来评估稳定性-指示质量。采用所提出的正相手性高效液相色谱法对D‐Valacyclovir杂质在原药和片剂剂型VAL中的释放度和稳定性进行了评价。
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引用次数: 2
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