气相色谱-串联质谱法测定有机肥料中6种痕量邻苯二甲酸酯  

Determination of 6 trace plasticizers in organic fertilizers by gas chromatography-tandem mass spectrometry

作　　者：潘扬昌[1] 莫达松[1] 何禹钦 盘杨桂 覃策焕 PAN Yangchang;MO Dasong;HE Yuqin;PAN Yanggui;QIN Cehuan(Guangxi Zhuang Autonomous Region Center for Analysis and Test Research,Nanning 530022,China;Guangxi Fuchuan Yao Autonomous County Water Supply Co.,Ltd,Fuchuan 542700,China;Guangxi Jinxiu Songyuan Forest Products Co.,Ltd,Jinxiu 545708,China)

机构地区：[1]广西壮族自治区分析测试研究中心,南宁530022 [2]广西富川瑶族自治县供水有限责任公司,广西富川542700 [3]广西金秀松源林产有限公司,广西金秀545708

出　　处：《化学分析计量》2025年第2期12-17,共6页Chemical Analysis And Meterage

基　　金：广西壮族自治区直属公益性科研院所基本科研业务费专项(2023ACZ01)。

摘　　要：建立了有机肥料中6种痕量邻苯二甲酸酯类残留的气相色谱-串联质谱检测方法。通过对样品处理参数的优化,确定了以正己烷-丙酮(体积比为1∶1)混合溶剂为提取溶剂,100 kHz功率超声波震荡提取30 min,旋转蒸发浓缩并将溶剂转换成正己烷,浓缩液经硅胶固相萃取小柱净化,使用15 mL正己烷-丙酮(体积比为8∶2)混合溶剂洗脱,洗脱液经旋转蒸发浓缩后再氮吹浓缩至1.00 mL以下,并用正己烷定容至1.00 mL。样品经气相色谱分离后,由三重四极杆串联质谱仪检测,采用多反应离子监测模式扫描,以保留时间及特征离子对定性,外标法定量。6种邻苯二甲酸酯类化合物在质量浓度2~500 ng/mL内与定量离子对色谱峰面积线性关系良好,相关系数为0.996~0.999 1,方法检出限为4~6μg/kg,加标回收率为74.33%~94.50%,测定结果的相对标准偏差为6.2%~13.4%(n=6)。该方法灵敏度高、准确、操作便捷,抗干扰强,适用于有机肥料中痕量的邻苯二甲酸酯类残留检测。A gas chromatography-tandem mass spectrometry method for the determination of six trace phthalates residues in organic fertilizers was established.Through the optimization of sample processing parameters,a mixed solvent of n-hexane acetone(volume ratio of 1:1)was determined as the extraction solvent,and the extractions was performed by ultrasonic oscillation at 100 kHz for 30 minutes.The solvent was concentrated by rotary evaporation and converted into n-hexane.The concentrated solution was purified by silica gel solid phase extraction column and eluted with 15 mL n-hexane-acetone(volume ratio of 8:2)mixed solvent.The eluent was concentrated by rotary evaporation and concentrated to less than 1.00 mL by nitrogen blowing,and then diluted to 1.00 mL with n-hexane.The samples were separated by gas chromatography,detected by triple quadrupole tandem mass spectrometer,and scanned by multi-reaction ion monitoring mode.Qualitative analysis was performed by retention time and characteristic ion pairs,and quantitative analysis was performed by external standard method.There was a good linear relationship between the mass concentration of 6 phthalate esters and the peak area of quantitative ion pair chromatography in the range of 2-500 ng/mL,the correlation coefficients were 0.996-0.9991.The detection limits were 4-6μg/kg,the recovery rate was 74.33%-94.50%,and the relative standard deviation of the test results was 6.2%-13.4%(n=6).The method is sensitive,accurate,easy to operate and anti-interference.It is suitable for the detection of trace phthalate residues in organic fertilizers.

关 键 词：气相色谱-串联质谱法 有机肥料 邻苯二甲酸酯 塑化剂 

分 类 号：O657.7[理学—分析化学]