Applicability of single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) using dwell times equal to or shorter than 100 μs has been tested for assessing titanium dioxide nanoparticles (TiO2 NPs) in bivalve mollusks. TiO2 NPs isolation from fresh mollusk tissues was achieved by ultrasound assisted enzymatic hydrolysis procedure using a pancreatin/lipase mixture. Optimum extraction conditions imply ultrasonication (60% amplitude) for 10 min, and 7.5 mL of a solution containing 3.0 g L-1of pancreatin and lipase (pH 7.4). The developed method was found to be repeatable (repeatability of 17% for the over-all procedure, TiO2 NPs concentration of 5.33 × 107 ± 8.89 × 106, n = 11), showing a limit of detection of 5.28 × 106 NPs g-1, and a limit of detection in size of 24.4-30.4 nm, based on the 3σ criteria, and on the 3σ/5 σ criteria, respectively. The analytical recovery within the 90-99% range (use of TiO2 NPs standards of 50 nm at 7 and 14 μg L-1 as Ti). Several bivalve mollusks (clams, cockles, mussels, razor clams, oysters and variegated scallops) were analyzed for total titanium (ICP-MS after microwave assisted acid digestion), and for TiO2 NPs by the proposed method. TiO2 NPs concentrations were within the 2.36 × 107-1.25 × 108 NPs g-1 range, and the most frequent sizes were from 50 to 70 nm.

中文翻译：

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在 sp-ICP-MS 之前超声辅助酶水解从双壳类软体动物中分离二氧化钛纳米颗粒

使用等于或短于 100 μs 的驻留时间的单粒子电感耦合等离子体质谱 (sp-ICP-MS) 的适用性已被测试用于评估双壳类软体动物中的二氧化钛纳米粒子 (TiO2 NP)。从新鲜软体动物组织中分离 TiO2 纳米颗粒是通过使用胰酶/脂肪酶混合物的超声辅助酶水解程序实现的。最佳提取条件意味着超声波处理（60% 振幅）10 分钟，以及 7.5 mL 含有 3.0 g L-1 胰酶和脂肪酶（pH 7.4）的溶液。发现开发的方法是可重复的（整个过程的重复性为 17%，TiO2 NPs 浓度为 5.33 × 107 ± 8.89 × 106，n = 11），显示检测限为 5.28 × 106 NPs g-1 ，以及基于 3σ 标准和 3σ/5 σ 标准的 24.4-30.4 nm 大小的检测限，分别。分析回收率在 90-99% 范围内（使用 50 nm 的 TiO2 NPs 标准，浓度为 7 和 14 μg L-1 作为 Ti）。使用建议的方法分析了几种双壳类软体动物（蛤、蛤、贻贝、蛏子、牡蛎和杂色扇贝）的总钛（微波辅助酸消解后的 ICP-MS）和 TiO2 纳米颗粒。TiO2 NPs 浓度在 2.36 × 107-1.25 × 108 NPs g-1 范围内，最常见的尺寸为 50 至 70 nm。