固相萃取–高效液相色谱法测定豆芽中4-氯苯氧乙酸钠和6-苄基腺嘌呤的残留量

建立了测定豆芽中4-氯苯氧乙酸钠和6-苄基腺嘌呤的固相萃取–高效液相色谱法。样品以0.1 mol/L的盐酸溶液为提取剂,经C18固相萃取柱净化处理,以乙腈–10 mmol/L乙酸铵水溶液(体积比25∶75)为流动相,Tech Mate C_(18)–ST色谱柱分离,4-氯苯氧乙酸钠和6-苄基腺嘌呤的紫外检测波长分别为228 nm和267 nm,色谱峰面积外标法定量。在0.50~100.00 mg/L浓度范围内,4-氯苯氧乙酸钠的相关系数为0.999 8,精密度在1.3%~8.2%之间(n=6),回收率在103.1%~109.0%之间;在0.05~10 mg/L浓度范围内,6-苄基腺嘌呤相关系数为0.999 9,精密度在0.9%~3.8%之间(n=6),回收率在88.0%~95.4%之间。4-氯苯氧乙酸钠和6-苄基腺嘌呤的检出限(S/N=3)分别为0.24,0.02 mg/kg。该法可以同时完成豆芽中4-氯苯氧乙酸钠和6-苄基腺嘌呤的分析检测。

Determination of Residual of 4-Chlorobenzene Sodium Acetate and 6-Benzyladenine in Bean Sprout by SPE-HPLC

The SPE-HPLC method for determination of 4-chlorobenzene sodium acetate and 6-benzyladenine in bean sprout was established. Samples were extracted with 0.1 mol/L hydrochloric acid and purified by C18 SPE column. The target compounds were separated by TechMate C18-ST column with acetonitrile-10 mmol/L ammonium acetate solution (25:75) as mobile phase. The UV detection wavelength of 4-chlorobenzene sodium acetate and 6-benzyladenine were 228 nm and 267 nm, respectively. The determinaion was performed by peak area with external standard method. The results showed that the linear range of 4-chlorobenzene sodium acetate was 0.5-100.00 mg/L with the linear correlation coefficients of 0.9998, RSD of determination results were 1.3%-8.2% and the recoveries were ranged from 103.1% to 109.0%; the linear range of 6-benzyladenine was 0.05-10 mg/L (n=6) with the linear correlation coefficients of 0.9999, RSD of determination results were 0.9%-3.8% (n=6) and the recoveries were ranged from 88.0% to 95.4%. The method detection limit of 4-chlorobenzene sodium acetate and 6-benzyladenine were 0.24 mg/kg and 0.02 mg/kg, respectively. The method can be used to analyze 4-chlorobenzene sodium acetate and 6-benzylaminopurin in bean sprouts at the same time.