Method Performance and Validation for Quantitative Analysis by 1H and 31P NMR Spectroscopy. Applications to Analytical Standards and Agricultural Chemicals

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• 作者：Grzegorz Maniara ; Kannan Rajamoorthi ; Srinivasan Rajan ; and Gerald W. Stockton
• 刊名：Analytical Chemistry
• 出版年：1998
• 出版时间：December 1, 1998
• 年：1998
• 卷：70
• 期：23
• 页码：4921 - 4928
• 全文大小：65K
• 年卷期：v.70,no.23(December 1, 1998)
• ISSN：1520-6882

文摘

Nuclear magnetic resonance (NMR) can be used toprovide an independent and intrinsically reliable determination of chemical purity. Unlike chromatography, itis possible to employ a universal reference standard asan internal standard for the majority of chemical productsassayed by quantitative NMR (QNMR). This is possiblebecause the NMR response can be made the same for allchemical components, including the internal standard, byoptimizing certain instrumental parameters. Experimentswere performed to validate the quantitative NMR methoddescribed in this paper for the analysis of organic chemicals. Experimental precision, accuracy, specificity, linearity, limits of detection and quantitation, and ruggedness were systematically addressed, and system suitabilitycriteria were established. The level of the major chemicalingredient can be determined with accuracy and precisionsignificantly better than 1%, and impurities may bequantified at the 0.1% level or below. Thus, QNMR rivalschromatography in sensitivity, speed, precision, andaccuracy, while avoiding the need for a reference standardfor each analyte. Examples are given of ¹H and ³¹P NMRused for quantitative analysis of agricultural chemicals,and a method for characterization of analytical standardsis presented.