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11.
Velusamy B. Subramanian Naresh Kumar Katari Thirupathi Dongala Sreekantha B. Jonnalagadda 《Biomedical chromatography : BMC》2020,34(1):e4719
A quality by design (QbD) based high-resolution HPLC method is described for determination of impurities in apixaban (APX) in the tablet dosage form. Employing a simple and stability-indicating HPLC method, nine known impurities were quantified with good peak resolution. Mobile phase A (MP-A) was prepared with buffer and acetonitrile 90:10 v/v, while mobile phase B (MP-B) contained water and acetonitrile 10:90 v/v. The gradient program was 0 min, MP-A 75%, B 25%; 20 min, MP-A 65%, B 35%; 30 min, MP-A 40%, B 60%; 40min, MP-A 40%, B 60%; 42 min, MP-A 75%, B 25%; and 50 min, MP-A 75%, B 25%. The chromatographic separation was achieved using a Zorbax RX C18 250 × 4.6 mm column, 5 μm (1.0 ml min−1, 280 nm, 50 μl) and a column temperature of 40°C. Several separation studies were carried out using design of experiments to optimize the method. Validation results confirm the applicability of the developed method for quality analysis and stability studies of the regular product on the manufacturing stream. 相似文献
12.
Prof. Yukishige Ito Prof. Yasuhiro Kajihara Prof. Yoichi Takeda 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(67):15461-15470
The introduction of Asn-linked glycans to nascent polypeptides occurs in the lumen of the endoplasmic reticulum of eukaryotic cells. After the removal of specific sugar residues, glycoproteins acquire signals in the glycoprotein quality control (GPQC) system and enter the folding cycle composed of lectin-chaperones calnexin (CNX) and calreticulin (CRT), glucosidase II (G-II), and UDP-Glc:glycoprotein glucosyltransferase (UGGT). G-II initiates glycoproteins’ entry and exit from the cycle, and UGGT serves as the “folding sensor”. This account summarizes our effort to analyze the properties of enzymes and lectins that play important roles in GPQC, especially those involved in the CNX/CRT cycle. To commence our study, general methods for the synthesis of high-mannose-type glycans and glycoproteins were established. Based on these, various substrates to analyze components of the GPQC were created, and properties of CRT, G-II, and UGGT have been clarified. 相似文献
13.
Vinod K. Ahirrao Rajiv A. Jadhav Suyog N. Vaidya Sachin S. Bhagwat Ravindra D. Yeole Mahesh V. Patel 《Biomedical chromatography : BMC》2022,36(6):e5354
Antibiotic susceptibility test (AST) discs are used as an in-vitro diagnostic tool to select the appropriate antibiotic to treat an infection. Generally, the concentration of the drug loaded on to the AST discs is measured by studying its activity against quality control organisms. This methodology has several limitations—it is time consuming, requires trained manpower, has a wider acceptance criteria of zone of inhibitions—causing ambiguity in judging smaller variations in drug concentration. To overcome these issues, we have developed and validated high-performance liquid chromatographic (HPLC) methods for the determination of strength of AST discs for in-house researched antibiotics, namely Levonadifloxacin/WCK 771, Nafithromycin/WCK 4873, Cefepime-Tazobactam/WCK 4282, and Cefepime-Zidebactam/WCK 5222. The drugs were extracted from the AST discs using an appropriate solvent. The developed methods are simple, accurate, precise, reproducible, rugged, and robust. They are efficient in terms of time, and can be easily conducted in a quality control laboratory during release as well as stability evaluation of AST disc. Application of HPLC methods for the determination of strength of AST discs ensures flawless quality and, consequently, a better selection of drugs to treat bacterial infections in clinics. 相似文献
14.
Influence of staff number and internal constellation on surgical site infection in an operating room
Prediction of bacteria-carrying particle (BCP) dispersion and particle distribution released from staffmem- bers in an operating room (OR) is very important for creating and sustaining a safe indoor environment. Postoperative wound infections cause significant morbidity and mortality, and contribute to increased hospitalization time. Increasing the number of personnel within the OR disrupts the ventilation airflow pattern and causes enhanced contamination risk in the area of an open wound. Whether the amount of staffwithin the OR influences the BCP distribution in the surgical zone has rarely been investigated. This study was conducted to explore the influence of the number of personnel in the OR on the airflow field and the BCP distribution. This was performed by applying a numerical calculation to map the airflow field and Lagrangian particle tracking (LPT) for the BCP phase. The results are reported both for active sampling and passive monitoring approaches. Not surprisingly, a growing trend in the BCP concentration (cfu/ms) was observed as the amount of staff in the OR increased. Passive sampling shows unpredictable results due to the sedimentation rate, especially for small particles (5-10 i~m). Risk factors for surgical site infections (SSls) must be well understood to develop more effective prevention programs. 相似文献
15.
Zhenguo Lv Guangzhe Yao Minglei Ge Yu Bai Mengxuan Wu Huizi Ouyang Jihong Feng Jun He 《Journal of separation science》2023,46(22):2300475
Physochlainae Radix (PR) is an essential herbal medicine that has been generally applied for treating cough and asthma. In this study, a comprehensive strategy for quality evaluation of PR from different origins was established by integrating qualitative identification, quantitative analysis, and chemometric methods. A total of 58 chemical components were identified by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF-MS/MS), and a sensitive and rapid UHPLC-QqQ-MS/MS method was established for the simultaneous determination of 12 compounds. In addition, multivariate statistical analysis was applied for discriminant analysis to compare the differences among 30 batches of PR samples. The results showed that the 30 batches of PR collected from four provinces could be clustered into three categories, in which scoparone, protocatechuic acid, tropic acid, and scopolin were important components to distinguish the primary and non-primary producing areas, as well as superior and inferior products of PR. Chemometric results were consistent and validated each other, and systematically explained the intrinsic quality characteristics of PR. This study first demonstrated that LC-MS combined with multivariate statistical analysis, provided a comprehensive and effective means for quality evaluation of PR. 相似文献
16.
Nina Wei Dandan Song Chang Lu Yong Jiang Qin Liu Lunyuan Liu Liu Xu Linwei Chen Zhipeng Chen 《Journal of separation science》2023,46(17):2300235
Aconitum carmichaelii is widely used to treat chronic and intractable diseases due to its remarkable curative effect, but it is also a highly toxic herb with severe cardiac and neurotoxicity. It has been combined with honey for thousands of years to reduce toxicity and enhance efficacy, but there has been no study on the chemical constituent changes in the honey-processing so far. In this study, the chemical constituents of A. carmichaelii before and after honey-processing were characterized by ultra-high-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry. The results showed that a total of 118 compounds were identified, of which six compounds disappeared and five compounds were newly produced after honey-processing, and the cleavage pathway of main components was elucidated. At the same time, 25 compounds were found to have significant effects on different products, among which four compounds with the biggest difference were selected for quantitative analysis by ultra-high-performance liquid chromatography-tandem mass spectrometry. This study not only explained the chemical differences between the different products, but also helped to control the quality of the honey-processed products more effectively, and laid a foundation for further elucidating the mechanism of chemical constituent change during the honey-processing of A. carmichaelii. 相似文献
17.
采用高效液相色谱法测定密胺餐具中的甲醛迁移量。样品经乙酸(4+96)溶液浸泡提取后,加入2,4-二硝基苯肼,与浸泡液中的甲醛反应生成2,4-二硝基苯腙,以C18色谱柱为分离柱,以甲醇-水(7+3)溶液为流动相进行等度洗脱,检测波长为350 nm。甲醛的质量浓度在0.01~40.0 mg·L-1范围内呈线性,测定下限(10S/N)为0.01 mg·L-1。对空白样品进行加标回收试验,回收率在99.8%~101%之间,相对标准偏差(n=10)均不大于0.6%。方法适用于密胺餐具中甲醛迁移量的检测。 相似文献
18.
W. Bamogo L. Mugherli A. Banyasz A. Novelli-Rousseau F. Mallard T.-H. Tran-Thi 《Analytica chimica acta》2015
A detection method for nicotinic acid, a specific metabolite marker of Mycobacterium tuberculosis present in cultures and patients' breath, is studied in complex solutions containing other metabolites and in biological media such as urine, saliva and breath condensate. The method is based on the analysis of the luminescence increase of Tb3+ complexes in the presence of nicotinic acid due to the energy transfer from the excited ligand to the lanthanide ion. It is shown that other potential markers found in M. tuberculosis culture supernatant, such as methyl phenylacetate, p-methyl anisate, methyl nicotinate and 2-methoxy biphenyl, can interfere with nicotinic acid via a competitive absorption of the excitation photons. A new strategy to circumvent these interferences is proposed with an upstream trapping of volatile markers preceding the detection of nicotinic acid in the liquid phase via the luminescence of Tb3+ complexes. The cost of the method is evaluated and compared with the Xpert MTB/RIF test endorsed by the World Health Organization. 相似文献
19.
Discrimination of crude and processed rhubarb products using a chemometric approach based on ultra fast liquid chromatography with ion trap/time‐of‐flight mass spectrometry 下载免费PDF全文
Min Wang Jinfeng Fu Huimin Guo Yuan Tian Fengguo Xu Rui Song Zunjian Zhang 《Journal of separation science》2015,38(3):395-401
Crude rhubarb subjected to different processing procedures will produce different therapeutic effects that are possibly due to processing‐induced variation in chemical composition. In this study, a chemometric approach based on ultra fast liquid chromatography with ion trap/time‐of‐flight mass spectrometry was established to systematically investigate the chemical variations of rhubarb induced by different processing methods. The approach was validated based on pooled quality‐control samples from two perspectives: the individual properties of variables and the bulk properties of samples. Orthogonal partial least squares discriminant analysis was introduced to compare the differences between crude and processed rhubarb products. A total of 20 significantly different markers were screened out and unambiguously/tentatively characterized. This research proved that a chemometric method based on ultra fast liquid chromatography with ion trap/time‐of‐flight mass spectrometry can comprehensively analyze the chemical variation of herbal medicine and provide evidence for a deeper understanding of the pharmacological activities of processed rhubarb products. 相似文献
20.
Analysis of ethyl glucuronide and ethyl sulfate using aqueous normal‐phase chromatography with mass spectrometry 下载免费PDF全文
The use of aqueous normal‐phase chromatography is explored as a possible format for the analysis of the forensically significant compounds ethyl glucuronide and ethyl sulfate. Standard solutions of the two compounds are used to verify the retention capabilities of two stationary phases (diamond hydride and undecanoic acid). These results are then compared to data obtained on hair extracts to determine if any matrix effects exist with respect to both retention and peak shape. The undecanoic stationary phase is used for the establishment of calibration curves for quantitative analysis. These curves are utilized to determine the concentration of ethyl glucuronide in several hair samples tested. 相似文献