全自动固相萃取—高效液相色谱法测定现制饮料中7种合成着色剂
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(1. 无锡市疾病预防控制中心〔南京医科大学附属无锡疾病预防控制中心〕,江苏 无锡 214023;2. 新疆克拉玛依市疾病预防控制中心,新疆 克拉玛依 834000;3. 无锡市食品安全检验检测中心,江苏 无锡 214142;4. 国家市场监管技术创新中心〔特殊食品〕,江苏 无锡 214142)

作者简介:

姚誉阳,男,无锡市疾病预防控制中心实验师,硕士。

通讯作者:

缪雄(1990—),男,无锡市食品安全检验检测中心检测工程师,学士。E-mail:751132516@qq.com薛强(1975—),男,无锡市疾病预防控制中心高级实验师,学士。E-mail:1477151962@qq.com

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基金项目:

无锡市卫生健康委重点学科项目(编号:LCZX2021006);新疆维吾尔自治区卫生健康青科项目(编号:WJWY-202307)


Determination of 7 synthetic colorants in freshly prepared beverages by high performance liquid chromatography dual wavelength method with automatic solid phase extraction
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(1. The Affiliated Wuxi Center for Disease Control and Prevention of Nanjing Medical University, Wuxi Center for Disease Control and Prevention,Wuxi, Jiangsu 214023, China; 2. Karamay City Center for Disease Control and Prevention, Karamay, Xinjiang 834000, China; 3. Wuxi Food Safety Inspection and Test Center, Wuxi, Jiangsu 214142, China; 4. Technology Innovation Center of Special Food for State Market Regulation, Wuxi, Jiangsu 214142, China)

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    摘要:

    目的:建立一种全自动固相萃取—高效液相色谱双波长法测定现制饮料中7种合成着色剂的方法。方法:样品经纯水提取2次,离心后,合并上清液,调节pH至3~4。利用全自动固相萃取装置活化Poly-sery色素专用固相萃取小柱,并上样、淋洗、洗脱。洗脱液氮吹浓缩至200 μL,用50%流动相A+50%流动相B混合液定容至1.0 mL。色谱柱采用C18柱,流动相为20 mmol/L乙酸铵—甲醇,梯度洗脱,流速1.0 mL/min,进样量10 μL,检测波长254,628 nm。结果:各物质在0.5~50.0 μg/mL范围内相关系数均大于0.999 9,方法检出限为0.023~0.179 mg/kg,定量限为0.078~0.598 mg/kg,加标回收率为92.4%~96.8%,相对标准偏差(RSD)为1.2%~4.2%。结论:该方法试剂使用量小,操作步骤简便,自动化程度高,回收率高,重复性好,适合于批量样品测定。

    Abstract:

    Objective: A method for the determination of 7 synthetic colorants in freshly prepared beverages by high performance liquid chromatography dual (HPLC) wavelength method with automatic solid phase extraction was established. Methods: Extraction conditions: The sample was extracted 2 times with pure water, and then the supernatant combined after centrifugation. The pH of the supernatant was adjusted to 3~4. After activation by an automatic solid-phase extraction device, loading, rinsing, and elution of the sample were carried out on the Poly-sery synthetic colorant solid-phase extraction column. The eluent was concentrated to 200 μL by nitrogen blowing, and then fixed to 1.0 mL with 50% mobile phase A+50% mobile phase B. Instrument conditions: The column was C18 column. The mobile phase was 20 mmol/L ammonium acetate-methanol, gradient elution. The flow rate was 1.0 mL/min. The injection volume was 10 μL. The detection wavelength were 254 nm and 628 nm. Results: The correlation coefficient of each substance in the range of 0.5~50 μg/mL was greater than 0.999 9, the detection limit of the method was 0.023~0.179 mg/kg, the quantitative limit was 0.078~0.598 mg/kg, the standard recovery was 92.4%~96.8%, and the relative standard deviation (RSD) was 1.2%~4.2%. Conclusion: This method has low consumption of toxic reagents, simple operation steps, high degree of automation, good recovery and repeatability, and it is suitable for the determination of large quantities of samples.

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姚誉阳,徐 曼,潘春燕,等.全自动固相萃取—高效液相色谱法测定现制饮料中7种合成着色剂[J].食品与机械,2024,40(3):82-88,94.
YAO Yuyang, XU Man, PAN Chunyan, et al. Determination of 7 synthetic colorants in freshly prepared beverages by high performance liquid chromatography dual wavelength method with automatic solid phase extraction[J]. Food & Machinery,2024,40(3):82-88,94.

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  • 收稿日期:2023-06-25
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  • 在线发布日期: 2024-04-30
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