Division of Food, Medicines and Consumer Safety, Section Medicinal Products, Scientific Institute of Public Health (WIV-ISP), J. Wytmansstraat 14, B-1050 Brussels, Belgium.
J Pharm Biomed Anal. 2012 Nov;70:64-70. doi: 10.1016/j.jpba.2012.05.022. Epub 2012 May 29.
A fast headspace GC-MS method was developed and validated for the detection and quantification of residual solvents of all three ICH-classes in counterfeit tablets and capsules. The method was validated for 10 solvents, selected based on an initial screening of counterfeit medicinal products. The considered solvents were ethanol, 2-propanol, acetone, ethylacetate, chloroform, carbon tetrachloride, benzene, toluene, dichloromethane and ethylbenzene. The proposed method uses a Phenomenex 624 capillary column (60 m × 0.32 mm; 1.8 μm film thickness) (Phenomenex, Torrance, USA) with an oven temperature program from 60 °C (held for 5 min) to 270 °C at 25 °C/min. 270 °C is held for 10 min. The total run time is 23.4 min. The obtained method was fully validated by applying the "total error" profile. Calibration lines for all components were linear within the studied ranges. The relative bias and the relative standard deviations for all components were smaller than 5%, the β-expectation tolerance limits did not exceed the acceptance limits of ±10% and the relative expanded uncertainties were acceptable for all of the considered components. A method was obtained for the screening and quantification of residual solvents in counterfeit tablets and capsules, which will allow a fast screening of these products for the presence of residual solvents.
建立并验证了一种快速顶空 GC-MS 方法，用于检测和定量假冒片剂和胶囊中所有三种 ICH 类别的残留溶剂。该方法针对基于对假冒药品的初步筛选选择的 10 种溶剂进行了验证。考虑的溶剂为乙醇、异丙醇、丙酮、乙酸乙酯、氯仿、四氯化碳、苯、甲苯、二氯甲烷和乙苯。所提出的方法使用 Phenomenex 624 毛细管柱（60 m×0.32 mm；1.8 μm 薄膜厚度）（Phenomenex，美国托伦斯），炉温程序从 60°C（保持 5 分钟）到 270°C，以 25°C/min 的速度升温。270°C 保持 10 分钟。总运行时间为 23.4 分钟。通过应用“总误差”曲线对获得的方法进行了全面验证。所有成分的校准曲线在研究范围内均呈线性。所有成分的相对偏差和相对标准偏差均小于 5%，β-期望公差限值未超过±10%的可接受限值，所有考虑成分的相对扩展不确定度均可接受。获得了一种用于筛查和定量假冒片剂和胶囊中残留溶剂的方法，该方法将允许快速筛查这些产品中残留溶剂的存在。
