摘要
目的建立甘蔗中3-硝基丙酸(3-NPA)的固相萃取-离子色谱检测方法。方法粉碎均质后甘蔗样品用乙腈涡旋振荡提取并离心,上清液经氨基固相萃取柱净化,15%甲醇氨洗脱,洗脱液氮吹浓缩后,纯水定容至5.00 ml,0.2μm微孔滤膜过滤,Dionex1500型离子色谱仪测定,选用AS19阴离子分析柱,10 mmol/L^20 mmol/L KOH溶液梯度淋洗,流速为1.00 ml/min,电导检测器检测。结果当3-硝基丙酸(3-NPA)的浓度为0.1μg/ml^10.0μg/ml时,线性关系良好,相关系数(r)为0.999 7,定性检出限(LOD)为0.03 mg/kg,定量检出限(LOQ)为0.10 mg/kg。2 g甘蔗样品加标2μg、10μg、50μg,得到的回收率为89.2%~98.4%,相对标准偏差(RSD)为2.24%~3.46%。结论该方法前处理过程操作简便、选择性强、净化效果好、回收率高,仪器响应灵敏,适用于针对甘蔗样品的食品安全监测和食物中毒分析。
Objective To develop a method for the determination of the 3- nitropropionic acid in sugarcane by solid phase extraction- ion chromatography. Methods The sugarcane samples were extracted with acetonitrile by vortex- assisted after homogenization and smash. Then the supernatant was purified by amino solid- phase extraction column and eluted with 15% ammonia water- methanol. The purified solution was concentrated by nitrogen,dissolved with pure water to 5. 00 ml and cleaned by0. 2 μm millipore filter. The ion chromatograph Dionex1500 with conductivity detector and AS19 analytical column were applied. The mobile phase was 10 mmol / L- 20 mmol / L KOH,and the flow rate was 1. 00 ml / min. Finally electrical conductivity detector was used for the detection. Results The calibration curves of 3- nitropropionic acid showed good linearity when the concentration was within 0. 1 μg / ml- 10. 0 μg / ml with correlation coefficient（ r） of 0. 999 7. The detection limits（ LOD） of the method was 0. 03 mg / kg,and the limits of quantification（ LOQ） was 0. 1 mg / kg. The spiked recoveries of three spiking levels（ 2 μg,10 μg and 50 μg） were within 89. 2%- 98. 4%,with the relative standard deviation within 2. 24%- 3. 46%. Conclusion This method has the advantages of simple operation,high selectivity,good purification effect,high recovery rate and sensitive instrument response. It is suitable for the analysis of food safety monitoring and food poisoning for sugarcane samples.
出处
《中国卫生检验杂志》
CAS
2016年第15期2154-2156,共3页
Chinese Journal of Health Laboratory Technology
基金
浙江省湖州市计划项目(2015GYB14)
关键词
固相萃取
离子色谱法
3-硝基丙酸
Solid phase extraction
Ion chromatography
3-nitropropionic acid
