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91.
Peptide bond‐forming reagents HOAt and HATU are not mutagenic in the bacterial reverse mutation test 下载免费PDF全文
John Nicolette Robin E. Neft Jessica Vanosdol Joel Murray 《Environmental and molecular mutagenesis》2016,57(3):236-240
The peptide bond‐forming reagents 1‐hydroxy‐7‐azabenzotriazole (HOAt, CAS 39968‐33‐7) and O‐(7‐Azabenzotriazol‐1‐yl)‐N,N,N′,N′‐tetramethyluronium hexafluorophosphate (HATU, CAS 148893‐10‐1) either have structural alerts, unclassified features or are considered out of domain when evaluated for potential mutagenicity with in silico programs DEREK and CaseUltra. Since they are commonly used reagents in pharmaceutical drug syntheses, they may become drug substance or drug product impurities and would need to be either controlled to appropriately safe levels or tested for mutagenicity. Both reagents were tested in the bacterial reverse mutation (Ames) test at Covance, under GLP conditions, following the OECD test guideline and ICH S2(R1) recommendations and found to be negative. Our data show that HOAt and HATU—common pharmaceutical synthesis reagents—are not mutagenic, and can be treated as ordinary drug impurities. Environ. Mol. Mutagen. 57:236–240, 2016. © 2016 Wiley Periodicals, Inc. 相似文献
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目的 采用改进的高效液相色谱法测定依帕司他原料药有关物质。方法 采用依利特Hypersil BDS C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-pH6.5磷酸盐缓冲液(0.025 mol·L-1 KH2PO4+0.025 mol·L-1 Na2HPO4,用H3PO4调节pH至6.5)为流动相,梯度洗脱,流速为1.0 mL·min-1,检测波长为396 nm和280 nm,柱温为30℃,进样量为20 μL。结果 依帕司他与相邻杂质能较好地分离。立体异构体杂质在浓度0.010~30 μg·mL-1内线性关系良好,检测限和定量限分别为0.80,2.4 ng·mL-1。精密度、稳定性、准确度、耐用性均符合要求。结论 该方法可用于依帕司他原料药有关物质的检查。 相似文献
94.
为了定量测定依卡倍特钠中潜在遗传毒性杂质依卡倍特磺酸乙酯(杂质Ⅰ),参考文献方法合成依卡倍特磺酸乙酯。采用高分辨质谱、结合二级质谱与核磁共振确定其相对分子质量及化学结构。采用Thermo C18色谱柱,以5 mmol/L乙酸铵溶液(甲酸调pH至3.0)为流动相A;乙腈为流动相B,按照梯度:0 min 50%B,4 min 50%B,12 min 80%B,16 min 80%B,16.1 min 50%B,20 min 50%B进行洗脱,柱温40 ℃;采用电喷雾负离子化-MS/MS选择反应监测。杂质Ⅰ的线性质量浓度范围为4~150 ng/mL,且线性关系良好(r=0.999);最低定量限为4 ng/mL;杂质Ⅰ的进样精密度、重复性和加标回收率良好,耐用性良好。方法操作简便,灵敏度高,可用于依卡倍特钠原料药中潜在遗传毒性杂质依卡倍特磺酸乙酯的含量测定。 相似文献
95.
Dina S. El-Kafrawy Ola H. El-Shoubashy Ahmed E. Issa Youssef A. Beltagy 《Sustainable Chemistry and Pharmacy》2022
Green analytical chemistry (GAC) is gaining great interest with the respect of global environmental pollution control (EPC). Consequently, we have developed two green chromatographic methods for the simultaneous precise and selective estimation of empagliflozin (EMP), linagliptin (LNA) with Metformin (MET) and its pharmacopoeial impurities cyanoguanidine (CGN) and melamine (MLN). The scientific database lacks any analytical reports tackling such concurrent estimation of the five cited analytes. The first developed method is a reversed phase HPLC-DAD employing Agilent C18 column (4.6 × 250 mm, 5 μm p.s.) and a mobile phase composed of methanol and 0.01 M sodium dihydrogen orthophosphate buffer of pH 2.55 (adjusted with orthophosphoric acid) eluted in a gradient mode with detection at 218 and 224 nm.The second method is HPTLC using Merk TLC plates precoated with 60 F 254 silica gel on aluminium sheet as the stationary phase developed with ethanol: ethylacetate: water (3.5: 3:1, v/v/v, respectively) as mobile phase and scanned at 216 and 224 nm. The proposed methods offered neat separation and quantitation of the five analytes in their pure form and in the triple combination tablets. Both methods were validated as per the ICH guidelines in terms of linearity, range, accuracy, precision, specificity and robustness. Moreover, Greenness assessment of the developed methods was carried out using the Analytical Eco-Scale. Further evaluation of the methods’ ecofriendliness and comparison with previously reported methods was performed using NEMI, GAPI and the novel AGREE tool. 相似文献
96.
确定2,6-二甲基苯胺为盐酸利多卡因注射液中遗传毒性杂质,N-氯乙酰-2,6-二甲基苯胺为潜在遗传毒性杂质,建立LC-MS/MS方法,用色谱柱Agilent ZORBAX Eclipse Plus C18(4.6 mm 250 mm,5 μm)对原料、自制制剂及原研制剂进行遗传毒性杂质研究。研究结果表明自制制剂中杂质2,6-二甲基苯胺与N-氯乙酰-2,6-二甲基苯胺除由原料引入外,可能分别由氧化条件或碱性条件下降解引入,为盐酸利多卡因注射液的遗传毒性风险评估和工艺优化提供参考与指导。 相似文献
97.
本试验建立了气相色谱串联质谱法测定苯甲酸阿格列汀中基因毒性杂质苯甲醛、苯甲醇、2-氰基溴苄和三正丁胺的分析方法。采用6%氰丙基苯-94%二甲基硅氧烷为固定相(DB-624,0.32 mm×30 m,1.8μm),用多反应监测模式检测。结果显示4种待测物均具有较好的线性关系,相关系数r≥0.9992,检测限均为2 ng/ml,平均回收率在90%~100%,且供试品溶液、杂质对照品溶液和系统适用性溶液在室温(25℃)放置12 h内稳定。3批生产规模样品中均未检出2-氰基溴苄、苯甲醛、苯甲醇和三正丁胺。说明本试验建立的分析方法灵敏度高、分离度好、结果准确,可有效分离并测定苯甲酸阿格列汀中的4种潜在毒性杂质,为其质量控制提供保障。 相似文献
98.
Beilin E Baker LJ Culbert P Toltl NP 《Journal of pharmaceutical and biomedical analysis》2008,46(2):316-321
A method for the quantification of acetol at mug/L levels in propylene glycol and glycerol, two common pharmaceutical excipients, was developed and validated. This simple yet highly specific method makes use of derivatization by O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBHA) in aqueous solution at room temperature followed by analysis via LC-MS without sample pre-concentration, extraction, or cleanup. Kinetic studies indicated that the derivatization reaction was complete after 4.5h. Preliminary investigations demonstrate the applicability of this method to the separation and identification of other electrophilic impurities. This suggests the potential for a simple, quantitative assay at room temperature in aqueous solution for the determination of a variety of electrophilic impurities in pharmaceutical excipients, without the need for sample concentration or extraction. 相似文献
99.
Nageswara Rao R Narasa Raju A Narsimha R 《Journal of pharmaceutical and biomedical analysis》2008,46(3):505-519
A reversed-phase high-performance liquid chromatographic method was developed for determination of process impurities and degradation products of bicalutamide in bulk drug and pharmaceutical formulations. The separation was accomplished on a Symmetry C(18) (4.6 mm x 250 mm; particle size 5 microm) column under isocratic mode. The mobile phase was 0.01 M KH(2)PO(4) (pH 3.0):acetonitrile (50:50 v/v) and a PDA detector set at 215 nm was used for detection. Forced degradation of bicalutamide was carried out under thermal, photo, acidic, alkaline and peroxide conditions. The unknown process impurities and alkaline degradation products were isolated and characterized by ESI-MS/MS, (1)H NMR and FT-IR spectral data. Under alkaline conditions bicalutamide was degraded in to an acid and an amine. The kinetics of degradation was studied. The proposed method was validated and successfully applied to the analysis of commercial formulations. Thus, the developed method can be used for process development as well as quality assurance of bicalutamide in bulk drug and pharmaceutical formulations. 相似文献
100.
目的 采用高效液相色谱-三重四极杆质谱法(LC-MS/MS)法测定替诺福韦酯前体药物中遗传毒性杂质9-丙烯基腺嘌呤含量,并分析最小二乘法不同线性拟合方法对结果准确度的影响。方法 采用Waters XBridge C18(4.6 mm×150 mm,3.5 μm)色谱柱;以甲醇-水(55:45)为流动相,流速:1.0 mL·min-1,等度洗脱8 min(2.0~2.6 min进质谱)。进样体积2 μL,柱温40 ℃。采用正离子电喷雾(ESI+)模式电离,多反应离子监测(MRM)模式,选择m/z 176.0→136.0作为检测离子。结果 经分析方法验证,该方法专属性良好;系统精密度试验RSD为1.1%(n=6);使用最小二乘法进行线性回归,线性范围0.051~25.250 μg·mL-1;加权线性回归在低浓度区域准确性明显高于未加权线性回归。定量限0.051 ng·mL-1,检出限0.017 ng·mL-1;原料药样品溶液平均回收率99.08%~99.97%(n=9),重复性RSD为0.4%~1.3%;片剂样品溶液平均回收率98.94%~101.96%(n=9),重复性RSD为0.2%~0.3%;耐用性良好。结论 建立的方法操作简单、灵敏度高、分析速度快、基质不影响检测,结果准确可靠,能够满足痕量遗传毒性杂质的检测要求。 相似文献