手性HPLC法测定R-(+)-2-(4-羟基苯氧基)丙酸的光学含量：DeterminationofchiralHPLC(+)R--2-(4-hydroxyphenoxy)propionicacidopticalcontent.docVIP

RP-HPLC内标法测定的含量 (国家精细化学品质量监督检验中心；泰州市产品质量监督检验所 泰州 225300) [摘要] 目的: 建立高效液相色谱法测定二氯喹啉酸钠盐含量的方法。方法：采用Agilent Eclipse XDB-C18 (50mm ×4. 6mm, 5μm)，柱温25 ℃，以甲醇：0.5%磷酸水(:40) 为流动相，流速为1.0mL·min-1，检测波长为2nm，进样体积10μL，按以峰面积计算二氯喹啉酸钠盐含量。结果: 在该色谱条件下二氯喹啉酸钠盐在～μg·mL-1范围内二氯喹啉酸钠盐色谱峰面积与其浓度成良好线性关系，R=为μg/mL（信噪比S/N＞10），检出限0.08μg/mL （信噪比S/N＞3）；平均回收率为%，RSD为%（n=6）。结论：该方法准确重复性好，二氯喹啉酸钠盐的。 [关键词] 二氯喹啉酸钠盐；高效液相色谱法；含量Determination of sodium uinclorac with high performance liquid chromatographic by using internal standard method CHEN Yan, QIAN Hui, WANG Aixia, HUANG Yinbo (China National Supervision Testing Center of fine Chemicals; Product Quality Supervising and Inspecting Institute of Taizhou City,,Taizhou 225300 ,China) Abstract: A high performance liquid chromatographic internal standard method with UV detection has been developed for the determination of sodium uinclorac. With diethylphthalate as internal standard method and uinclorac as reference substances. The chromatographic separation was achieved on a reversed phase C18 column with the mobile phase of methanol/water mixture of 0.5% phosphoric acid (60:40, v/v) at a flow rate of 1.0mL/min. The UV detection wavelength was set at 230nm and the column temperature was set at 25℃ with 10μL injection volume. The calibration curve was good linear over the of 21.5～μg·mL-1 and the linear correlation coefficient was 0.9999(n=6); The lower limit of quantificantion was 0.2μg/mL(S/N＞10μg/Ml(S/N＞3)% with RSD=1.14%. The results showed that method Is accurate and precise with lower threshold.Therefore, which is applicable to detect the sodium uinclorac . Keywords: sodium uinclorac; HPLC; herhicide ; internal standard method; content 二氯喹啉酸二氯喹啉酸是防除稻田稗草的特效选择性除草剂，属激素型喹啉羧酸类除草剂，杂草中毒症状与生长素类作用相似，主要用于防治稗草且适用期长，1-7叶期均有效，颇受商家、农户青睐。近年来随着使用二氯喹啉酸趋多，陆续出现一些问题，多次引起农户投诉或纷争，二氯喹啉酸[1-4]，但诸多关于二氯喹啉酸的方法研究及方法验证略显粗糙简单，如Liu和Wang等人[1-3]报道了采用高效液相外标法对二氯喹啉酸[1-4]未给出方法的定量限、最低检出限、稳定性等重要数据的考察。由于内标法能校准和消除操作条件的波动对分析结果产生的影响，[4-7]的基础上,用高效液相色谱内标法对二氯喹啉酸钠盐的含量检测方法进行系统全面的研究与验证，为有效控制二氯喹啉酸二氯喹啉酸实验部分 1.1