QuEChERS-气相色谱-串联质谱法测定辣椒油树脂中16种邻苯二甲酸酯及其影响因素探究  

Determination of 16 phthalates in capsicum oleoresin by QuEChERS and gas chromatography-mass spectrometry and its influencing factors

作　　者：张杰 钱建瑞 王丽沙 张玉芬 吴迪 连运河 ZHANG Jie;QIAN Jianrui;WANG Lisha;ZHANG Yufen;WU Di;LIAN Yunhe(Chenguang Biotech Group Co.,Ltd.,Handan 057250;Chenguang Biotech Group of Handan,Handan 057250;Natural Pigment Industry Research Institute of Hebei,Handan 057250)

机构地区：[1]晨光生物科技集团股份有限公司,邯郸057250 [2]晨光生物科技集团邯郸有限公司,邯郸057250 [3]河北省植物天然色素产业技术研究院,邯郸057250

出　　处：《中国食品添加剂》2023年第10期262-269,共8页China Food Additives

基　　金：河北省创新能力提升计划项目(205676100H)。

摘　　要：本文采用QuEChERS技术结合气相色谱-质谱(GC-MS)技术,建立了辣椒油树脂中16种邻苯二甲酸酯(PAEs)定量分析方法。由于辣椒油树脂基质复杂,通过探究提取试剂、提取方式及净化材料用量及配比,最终建立起适合辣椒油树脂的QuEChERS前处理方式。以16种邻苯二甲酸酯在不同极性溶剂(正己烷、异辛烷、乙酸乙酯、乙腈)中的回收率为考核指标,最终确定乙腈作为提取溶剂,并在2000 r/min下涡旋3 min得以充分提取。综合比较考虑石墨化炭黑(GCB)、十八烷基键合硅胶(C18)、乙二胺-N-丙基硅烷(PSA)、硅胶(Silica)对16种邻苯二甲酸酯的吸附作用和对辣椒油树脂基质的净化效果,选择PSA、Silica(300 mg+300 mg)进行样品净化,并在选择离子监测模式(SIM)下进行定量分析。结果表明,提取试剂和净化材料的选择及用量配比,是影响检测结果的关键直接因素。16种PAEs质量浓度在0.015~1.0 mg/kg范围内具有较好的线性相关性(R^(2)>0.9990);其中,辣椒油树脂中16种邻苯二甲酸酯的检出限(LODs)在0.186~4.080μg/kg之间,样品加标回收率在83.9%~108.2%之间,相对标准偏差<10%(n=6)。该方法可操作性强、重现性好,灵敏度、准确度和精密度高,适用于辣椒油树脂中PAEs残留的快速批量检测。A precise quantitative analysis method for phthalate esters(PAEs)in capsicum oleoresin was established using QuEChERS combined with GC-MS.Because of complex matrix of capsicum oleoresin,it is necessary to explore extraction reagent and procedure,various kinds of decontaminant to establish an appropriate pretreatment method for capsicum oleoresin.Take the recoveries of 16 PAEs in different polarity solvents into account,ultimately,acetonitrile was selected for targets extraction.In light of adsorption of GCB,C18,PSA,Silica for 16 PAEs and purification capacity for capsicum oleoresin,the capsicum oleoresin were purified with PSA、Silica(300 mg+300 mg).The quantitative analysis was carried out under selective ion monitoring(SIM).The results showed that the extraction reagent and types of purification materials act as core factors which showed direct influence on the detect of 16PAEs.The 16 PAEs had good linear correlation in the concentration range of 0.015〜1.0 mg/kg(R^(2)>0.9990).The limits of detection(LODs)of capsicum oleoresin were in the range of 0.186〜4.080μg/kg,and the recoveries of 16 PAEs varies from 83.9% to 108.2% with relative standard deviations(RSDs)lower than 10%.The method was applicable and reproducible with good sensitivity,accuracy and precision,which could be used for quantitative determination of phthalate esters in capsicum oleoresin.

关 键 词：气相色谱-质谱法(GC-MS) 辣椒油树脂 邻苯二甲酸酯 QUECHERS 

分 类 号：TS202.3[轻工技术与工程—食品科学] O652.1[轻工技术与工程—食品科学与工程]