An analytical method was developed for the quantification of spinosad (sum of spinosyns A and D) in five animal‐derived products (chicken breast, pork, beef, egg, and milk) using LC–MS/MS. The sample was extracted using acetonitrile/1% acetic acid and a combination of magnesium sulfate and sodium acetate salts. The sample was purified using multiwalled carbon nanotubes as sorbent via a dispersive‐solid‐phase extraction procedure. Matrix‐matched calibration (seven‐point) provided good linearity with coefficient of determination (R²) ≥0.99 for each product. The limits of detection and quantification (LOQs) ranged between 0.0003–0.03 and 0.001–0.1 mg/kg, respectively. Method validation was carried out after spiking the target standard to blank matrices at the concentration levels of LOQ, 2 × LOQ, and 10 × LOQ with three replicates for each. The average recoveries were between 74 and 104%, with relative standard deviations ≤9.68, which were within the acceptable range designated by the international organizations. The developed method was successfully applied for monitoring market samples collected throughout the Korean Peninsula, and none of the samples tested positive for the target analytes. It has therefore been shown that dehydration and acidification were effective to extract spinosad from animal‐derived products.

中文翻译：

---

使用多壁碳纳米管结合LC-MS / MS进行动物衍生产品中多杀菌素A和多杀菌素D的定量分析

开发了一种使用LC-MS / MS定量分析五种动物源性产品（鸡胸肉，猪肉，牛肉，鸡蛋和牛奶）中的多杀菌素（多杀菌素A和D的总和）的分析方法。使用乙腈/ 1％乙酸以及硫酸镁和乙酸钠盐的混合物萃取样品。通过分散固相萃取程序，使用多壁碳纳米管作为吸附剂纯化样品。矩阵匹配的校准（七点）具有良好的线性和测定系数（R ²）每种产品≥0.99。检出限和定量限（LOQs）分别在0.0003–0.03和0.001–0.1 mg / kg之间。在将目标标准品加标到空白基质中，浓度分别为LOQ，2×LOQ和10×LOQ时，进行方法验证，每次重复三次。平均回收率在74％至104％之间，相对标准偏差≤9.68，在国际组织指定的可接受范围内。所开发的方法已成功应用于监测整个朝鲜半岛的市场样品，并且没有一个样品的目标分析物呈阳性。因此表明，脱水和酸化可有效地从动物源性产品中提取多杀菌素。