UHPLC-MS/MS法同時測定調味品中5種脂溶性色素和5種罌粟殼生物堿的殘留量

摘要：建立了一種經QuEChERS EMR（Enhanced Matrix Removal）-Lipid凈化結合超高效液相色譜-串聯質譜（UHPLC-MS/MS）同時測定調味品中蘇丹紅Ⅰ～Ⅳ、對位紅5種脂溶性色素和罌粟堿、嗎啡、可待因、蒂巴因、那可丁5種罌粟殼生物堿殘留量的高通量分析方法。罌粟堿、蒂巴因、那可丁和5種脂溶性色素在1～100 ng/mL范圍內線性關系良好，相關系數均大于0.99，定量限（LOQ）為1.0 μg/kg；嗎啡、可待因在8～100 ng/mL范圍內線性關系良好，相關系數均大于0.99，定量限（LOQ）為5.0 μg/kg；各化合物平均回收率為81.2%～104.5%，相對標準偏差為2.9%～11.4%（n=6）。該方法簡便、靈敏、穩定、通量高、成本低，適用于香辛料調味油、火鍋底料及蘸料、麻辣燙底料等多種調味品的檢測質控需求。

關鍵詞：QuEChERS EMR-Lipid；超高效液相色譜-串聯質譜；脂溶性色素；罌粟殼生物堿；調味品

中圖分類號：TS201.2""""" 文獻標志碼：A"""" 文章編號：1000-9973（2024）10-0179-07

Simultaneous Determination of Residual Amount of Five Lipid Soluble Pigments

and Five Poppy Husk Alkaloids in Seasonings by UHPLC-MS/MS Method

DING Wen-hui1， TIAN Hong-xia1， ZHU Wei-wei1， ZHANG Shuai2

（1.School of Food and Drug， Weifang Vocational College， Weifang 261000， China;

2.Anqiu Inspection and Testing Center Co.， Ltd.， Weifang 262100， China）

Abstract： A high-throughput analysis method is established for the simultaneous determination of residual amount of five lipid soluble pigments such as Sudan Red Ⅰ～Ⅳ and Para Red， as well as five poppy husk alkaloids such as papaverine， morphine， codeine， thebaine and narcotine in seasonings using QuEChERS EMR （Enhanced Matrix Removal）-Lipid purification combined with ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS）. Papaverine， thebaine， narcotine and five lipid soluble pigments show a good linear relationship within the range of 1～100 ng/mL， the correlation coefficients are all greater than 0.99， and the limit of quantification （LOQ） is 1.0 μg/kg.Morphine and codeine show a good linear relationship within the range of 8～100 ng/mL， the correlation coefficients are both greater than 0.99， and the limit of quantification （LOQ） is 5.0 μg/kg. The average recovery rates of each compound range from 81.2% to 104.5%， with the relative standard deviations between 2.9% and 11.4% （n=6）.The method is simple， sensitive， stable， high-throughput and low-cost， and it is suitable for the detection and quality control requirements of various seasonings such as" spice flavored oil， hotpot seasoning and dipping sauce， and Malatang seasoning.

Key words： QuEChERS EMR-Lipid; UHPLC-MS/MS; lipid soluble pigments; poppy husk alkaloids; seasoning

蘇丹紅Ⅰ～Ⅳ、對位紅是脂溶性偶氮類工業染料，禁止用于食品染色。蘇丹紅及其代謝產物具有致癌性、遺傳毒性、致敏性；對位紅對眼睛、皮膚和呼吸系統有刺激性，其毒性尚不明確。由于此類染料廉價易得、著色穩定、添加后產品鮮艷光亮，故仍有不法商家在調味品中使用。罌粟殼生物堿屬于非食用違禁物質，長期食用會對人體神經系統、消化系統造成損害。根據整頓辦函[2011]1號和食品整治辦[2008]3號文件的要求：食品中不得檢出蘇丹紅Ⅰ～Ⅳ和罌粟殼生物堿成分。因此，建立一種先進且通用易行的檢測方法是十分必要的。

蘇丹紅Ⅰ～Ⅳ、對位紅的檢測方法有薄層色譜法[1]、液相色譜法 [2-4]和液相色譜-串聯質譜法 [5-6]；罌粟殼生物堿的檢測方法有氣相色譜-質譜法[7]、液相色譜-串聯質譜法[8-10]。……