光电二极管阵列离子对高效液相色谱法测定米豆腐中溴酸盐的含量

Determination of bromate in rice tofu by ion-pair high performance liquid chromatography with photodiode array detector

中文关键词:  米豆腐  溴酸盐  离子对  光电二极管阵列检测  高效液相色谱法

英文关键词:rice tofu  bromate  ion-pair  photodiode array detector  high performance liquid chromatography

中文摘要:

      目的 建立光电二极管阵列离子对高效液相色谱法测定米豆腐中溴酸盐的方法。方法 用水作溶剂超声提取米豆腐中溴酸盐, 提取液浓缩后用流动相溶解。经Waters C18色谱柱(250 mm×4.6 mm, 5 μm), 以 0.5 mmol/L十二烷基三甲基氯化铵溶液-甲醇(80:20, V:V)洗脱, 流速为1.0 mL/min, 柱温30 ℃, 以保留时间和光谱图定性, 以210 nm处的吸光度定量。结果 溴酸盐在1.00~100 μg/mL范围内线性关系良好, 相关系数r2=0.9997 (n=6), 平均加标回收率为91.3%~96.1%, 相对标准偏差(relative standard deviation, RSD)为0.8%~ 0.9%。检出限(limit of detection, LOD)与定量限(limit of quantification, LOQ)分别为0.7、2.0 mg/kg。 结论 该法操作简单, 定量准确, 专属性强, 可用于米豆腐中溴酸盐的检测。

英文摘要:

      Objective To establish a method for determination of bromate in rice tofu by ion-pair high performance liquid chromatography with photodiode array detector. Methods Bromate in rice tofu was extracted with water as solvent by ultrasonic. The extraction was concentrated and dissolved with mobile phase. Samples were separated on a Waters C18 column (250 mm × 4.6 mm, 5 μm), eluted with 0.5 mmol/L dodecyltrimethylammonium chloride solution-methanol (80:20, V:V) at a flow rate of 1.0 mL. /min, column temperature 30 ℃, retention time and spectrogram were used for the qualitative determination and the absorbance at 210 nm was used for quantitative determination. Results The calibration curve was linear in the range of 1.00 to 100 μg/mL and the correlation coefficient was 0.9997 (n=6), the average recoveries were 91.3%-96.1%, and the relative standard deviation (RSD) were 0.8%-0.9%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.7 and 2.0 mg/kg, respectively. Conclusion This method is simple, accurate, and reliable, which is suitable for the determination of bromate in rice tofu.