酶提取-单颗粒电感耦合等离子质谱法分析樱桃番茄纳米银颗粒及其吸收规律研究

Study on the Absorption of Silver Nanoparticlesin Cherry Tomatoes by Single Particle Inductively Coupled Plasma Mass Spectrometry with Enzyme Extraction

为探究复合保鲜涂膜中AgNPs的迁移情况,采用酶提取的前处理方式,结合单颗粒电感耦合等离子体质谱(SP-ICP-MS)法,考察了前处理方式、驻留时间、校准方式以及Ag^(+)浓度等条件对AgNPs准确测定的影响。结果表明:0.1 g樱桃番茄样品在柠檬酸盐体系下使用0.2 g R-10离析酶可达到消解最适酶剂量;当驻留时间小于100μs时,测定结果有较好的积分条件以及较高的信背比;采用AgNP尺寸方式进行校准比单独用Ag^(+)标准溶液校准方式的颗粒尺寸测定结果更加准确。方法用来测定樱桃番茄中加标AgNPs颗粒回收率达到88.9%,粒径实测值为(47.8±0.3) nm,粒径检出限为13 nm,颗粒浓度检出限为7.5×10~4 particles/L。通过将樱桃番茄暴露于AgNPs涂膜中来探究AgNPs迁移行为,复合保鲜涂膜后的樱桃番茄通过三次洗涤后能够在表面去除大部分AgNPs,但仍有少量AgNPs穿过果表皮浸入果肉组织。方法灵敏度高,操作简单,能够为揭示AgNPs在农产品及农业生产中的风险提供可靠、准确的表征方法。

In order to investigate the migration of AgNPs in the composite freshness coating film,the pretreatment of enzyme extraction combined with single particle inductively coupled plasma mass spectrometry(SP-ICP-MS)were used to investigate the effects of pretreatment,residence time,calibration method and Ag+concentration on accurate determination of AgNPs.The results showed that the optimal enzyme dosage of 0.1 g of sainfoin sample in citrate system with 0.2 g R-10 dissociating enzyme could reach the optimal enzyme dosage for the dissociation.When the residence time was less than 100μs,the results showed better integration conditions and higher signal-to-back ratios.Compared with the method of AgNPs particle size calibration using Ag+standard solution,the accuracy of AgNPs particle size calibration was higher.When the concentration of Ag+was greater than 0.2μg/kg,the calibration result of this method was better than that of the calibration method using Ag+standard solution alone.When the concentration of Ag+was greater than 0.2μg/L,it affected the determination of AgNPs less than 30 nm,and therefore,dilution was required to verify the accuracy of the measured AgNPs particle size.The recovery of spiked AgNPs particles in the saint′s fruits was 88.9%,the measured particle size was(47.8±0.3)nm,the detection limit of particle size was 13 nm,and the detection limit of particle concentration was 7.5×104 particles/L.The migration behaviors of AgNPs were investigated by exposing the saint′s fruits to the AgNPs coated film,and the saint′s fruits with composite freshness coating were able to remove a large amount of AgNPs through three washes.After three washes,a large amount of AgNPs were removed,but a small amount of AgNPs still leached into the pulp tissue through the fruit epidermis.The method is highly sensitive and simple to operate,and can provide a reliable and accurate characterization method for revealing the risk of AgNPs in agricultural products and agricultural production.