顶空/气相-质谱法测定蔬菜中顺(反)-1,3-二氯丙烯含量

Determination of cis(trans)-1,3-dichloropropene in vegetable by headspace gas chromatography-mass spectrometry

目的建立顶空/气相色谱质谱法测定蔬菜中顺(反)-1,3-二氯丙烯含量。方法样品中加入饱和NaCl溶液(磷酸调pH小于2),利用顶空/气相色谱质谱法检测顺(反)-1,3-二氯丙烯含量。结果在质量浓度为0.1~10μg/L范围内,顺(反)-1,3-二氯丙烯线性相关系数r2分别为0.9999、0.9997,检出限为2μg/kg。顺(反)-1,3-二氯丙烯添加水平在0.4~40μg/kg范围内,6次重复的平均添加回收率分别为93.98%~117.68%和93.92%~98.23%,相对标准偏差分别为3.49%~8.14%和1.15%~9.72%。结论该方法准确度高、精密度良好,符合分析测试质控要求。

Objective To establish a method for the determination of cis(trans)-1,3-dichloropropene in vegetables by headspace gas chromatography-mass spectrometry.Methods Saturated NaCl solution(pH adjusted by phosphoric acid was less than 2)was added into the sample,and the content of cis(trans)-1,3-dichloropropene was detected by headspace gas chromatography-mass spectrometry.Results When the concentration range was 0.1-10μg/L,the correlation coefficient of cis(trans)-1,3-dichloropropene were 0.9999 and 0.9997 respectively,and the limit of detection was 2μg/kg.The average recoveries were 93.98%-117.68%and 93.92%-98.23%,and the relative standard deviations were 3.49%-8.14%and 1.15%-9.72%respectively,at fortified concentration range of 0.4-40μg/kg.Conclusion This method has high accuracy and good precision,which meets the requirements of quality control of analysis and test.