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核磁共振波谱内标法测定四氯虫酰胺标样的含量

作  者:
郎洁;董燕;王嫱;杨辉斌;于海波
单  位:
关键词:
四氯虫酰胺;定量核磁共振;内标法;含量测定
摘  要:
[目的]采用核磁共振波谱内标法,建立了快速、专属、准确测定四氯虫酰胺标样含量的方法。[方法]使用日本电子公司JNM-ECZ600R超导核磁共振波谱仪,以氘代二甲基亚砜为溶剂,顺丁烯二酸为内标,在测定温度25℃、脉冲宽度8.0μs、延迟时间为5 s、扫描次数8的条件下采集样品氢谱。[结果]以化学位移δ分别为10.55和6.27的四氯虫酰胺和顺丁烯二酸的氢质子峰作为定量峰,其峰面积比y(As/Ar)与质量比x(ms/mr)进行线性回归,相关系数为0.9999。含量测定重复性试验的RSD值为0.38%,稳定性的RSD值为0.77%,测得四氯虫酰胺标样的含量为99.6%。[结论]在没有标准对照品的情况下,核磁共振波谱法可用于四氯虫酰胺的含量测定,该方法具有快速、准确、简便的优点。
译  名:
Quantitive Determination of Tetrachlorantraniliprole by ~1H NMR Spectroscopy with Internal Standard Method
作  者:
LANG Jie;DONG Yan;WANG Qiang;YANG Hui-bin;YU Hai-bo;State Key Laboratory of the Discovery and Development of Novel Pesticide,Shenyang Sinochem Agrochemicals R&D Co.,Ltd.;
关键词:
tetrachlorantraniliprole;;qNMR;;internal standard method;;quantitive determination
摘  要:
[Aims] This study aims to establish a rapid, specific and simple method for the quantitive determination of tetrachlorantraniliprole by ~1H NMR. [Methods]~1H NMR spectroscopy was acquired in DMSO, scanning 8 times at 25 ℃ with a Jeol JNM-ECZ600R, pulses width 8.0 μs,delay time 5 s, and maleic acid as internal standard. [Results] The integration of proton signals at δ 10.55 for tetrachlorantraniliprole and at δ 6.27 for maleic acid was used for quantification. The correlation coefficient was 0.9999 for quantitative peak areas ratio y(As/Ar) of tetrachlorantraniliprolemaleic acid versus mass ratio x(ms/mr). The precision RSD was 0.38%, the stability RSD was 0.77%. The contents of tetrachlorantraniliprole was 99.6%. [Conclusions] The results showed that ~1H NMR method can be used for the quantative determination of tetrachlorantraniliprole with reference substance. The method is rapid, accurate and simple.

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