Bekiroglu Somer, Myrberg Olle, Ostman Kristina, Ek Marianne, Arvidsson Torbjörn, Rundlöf Torgny, Hakkarainen Birgit
Division of Analytical Pharmaceutical Chemistry, Department of Medicinal Chemistry Uppsala University, Biomedical Centre, P.O. Box 574, SE-751 23 Uppsala, Sweden.
J Pharm Biomed Anal. 2008 Aug 5;47(4-5):958-61. doi: 10.1016/j.jpba.2008.03.021. Epub 2008 Mar 28.
A 1H-nuclear magnetic resonance (NMR) spectroscopy method for quantitative determination of benzethonium chloride (BTC) as a constituent of grapefruit seed extract was developed. The method was validated, assessing its specificity, linearity, range, and precision, as well as accuracy, limit of quantification and robustness. The method includes quantification using an internal reference standard, 1,3,5-trimethoxybenzene, and regarded as simple, rapid, and easy to implement. A commercial grapefruit seed extract was studied and the experiments were performed on spectrometers operating at two different fields, 300 and 600 MHz for proton frequencies, the former with a broad band (BB) probe and the latter equipped with both a BB probe and a CryoProbe. The concentration average for the product sample was 78.0, 77.8 and 78.4 mg/ml using the 300 BB probe, the 600MHz BB probe and CryoProbe, respectively. The standard deviation and relative standard deviation (R.S.D., in parenthesis) for the average concentrations was 0.2 (0.3%), 0.3 (0.4%) and 0.3mg/ml (0.4%), respectively.
开发了一种用于定量测定作为葡萄柚籽提取物成分的苄索氯铵（BTC）的1H核磁共振（NMR）光谱法。该方法经过验证，评估了其特异性、线性、范围、精密度以及准确度、定量限和稳健性。该方法包括使用内参标准物1,3,5-三甲氧基苯进行定量，被认为简单、快速且易于实施。对一种市售葡萄柚籽提取物进行了研究，并在质子频率分别为300和600 MHz的两种不同磁场的光谱仪上进行了实验，前者配备宽带（BB）探头，后者配备BB探头和低温探头。使用300 BB探头、600 MHz BB探头和低温探头时，产品样品的浓度平均值分别为78.0、77.8和78.4 mg/ml。平均浓度的标准偏差和相对标准偏差（R.S.D.，括号内）分别为0.2（0.3%）、0.3（0.4%）和0.3 mg/ml（0.4%）。
