Validation of a quantitative NMR method for suspected counterfeit products exemplified on determination of benzethonium chloride in grapefruit seed extracts
Validation of a quantitative NMR method for suspected counterfeit products exemplified on determination of benzethonium chloride in grapefruit seed extracts
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DOI：
10.1016/j.jpba.2008.03.021
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发表时间：
2008-08-05
影响因子：
3.4
通讯作者：
Hakkarainen, Birgit
中科院分区：
文献类型：
--
作者：
Bekiroglu, Somer;Myrberg, Olle;Hakkarainen, Birgit
建立了一种h -1核磁共振（NMR）光谱法定量测定葡萄柚籽提取物中苯并索氯铵（BTC）的方法。对该方法进行了验证，评估了其特异性、线性度、范围和精密度，以及准确度、定量限和鲁棒性。该方法采用内参标准品1,3,5-三甲氧基苯进行定量，简便、快速、易于实施。以商品葡萄柚籽提取物为研究对象，在质子频率为300和600 MHz的两个不同领域的光谱仪上进行了实验，前者配备了宽带（BB）探针，后者配备了BB探针和低温探针（TM）。使用300 BB探针、600 MHz BB探针和CryoProbe (TM)，产品样品的平均浓度分别为78.0、77.8和78.4 mg/ml。平均浓度的标准偏差为0.2(0.3%)，相对标准偏差为0.3(0.4%)，相对标准偏差为0.3 mg/ml（0.4%）。(c) 2008 Elsevier B.V.版权所有
A H-1-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 (TM). The concentration average for the product sample was 78.0, 77.8 and 78.4 mg/ml using the 300 BB probe, the 600 MHz BB probe and CryoProbe (TM), 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 0.3 mg/ml (0.4%), respectively. (c) 2008 Elsevier B.V. All rights reserved.