He Limin, Su Yijuan, Fang Binghu, Shen Xiangguang, Zeng Zhenling, Liu Yahong
Department of Pharmacology and Toxicology, College of Veterinary Medicine, South China Agricultural University, Guangzhou, Guangdong PC 510642, PR China.
Anal Chim Acta. 2007 Jun 26;594(1):139-46. doi: 10.1016/j.aca.2007.05.021. Epub 2007 May 21.
A sensitive and cheap high performance liquid chromatography (HPLC) with ultraviolet-visible (UV-VIS) was developed for the determination of Sudan dyes (I, II, III, and IV) residues in various types of eggs. The chromatographic separation was achieved on a reverse phase C18 column with gradient elution, using a mobile phase of 0.1% formic acid acetonitrile/0.1% formic acid aqueous solution; detector was set at 478 nm for Sudan I and 520 nm for Sudan II, III and IV. The suspected egg samples were derivatized with N,O-bis (trimethylsilyl) trifluoro-acetamide and confirmed by gas chromatography-mass spectrometry (GC-MS) in EI. Mass spectra of trimethylsilyl derivatives of the Sudan dyes were built up in EI mode. Recoveries of the Sudan dyes ranged between 79.8 and 95.7% in eggs by HPLC-UV, with all the relative standard deviations of less than 5%. Limit of detection (LOD), limit of quantification (LOQ) were in the range of 4.0-4.8 and 12.3-13.8 microg kg(-1) in eggs, respectively. Identification and confirmation could be validated in the range of 2.0-4.2 microg kg(-1) with the GC-MS method. This method is suitable for routine fast monitoring, screening and confirmation of Sudan dyes residues in eggs, as mandated by regulatory agencies.
建立了一种灵敏且廉价的高效液相色谱法（HPLC）结合紫外可见（UV-VIS）检测技术，用于测定各类鸡蛋中苏丹红染料（I、II、III和IV）的残留量。采用反相C18柱，以0.1%甲酸乙腈/0.1%甲酸水溶液为流动相进行梯度洗脱，实现色谱分离；检测波长设定为苏丹红I 478 nm，苏丹红II、III和IV 520 nm。可疑鸡蛋样品用N，O-双（三甲基硅基）三氟乙酰胺进行衍生化处理，并通过气相色谱-质谱联用仪（GC-MS）在电子轰击（EI）模式下进行确证。建立了苏丹红染料三甲基硅基衍生物在EI模式下的质谱图。通过HPLC-UV测定鸡蛋中苏丹红染料的回收率在79.8%至95.7%之间，相对标准偏差均小于5%。鸡蛋中苏丹红染料的检测限（LOD）和定量限（LOQ）分别在4.0 - 4.8和12.3 - 13.8 μg kg⁻¹范围内。采用GC-MS方法在2.0 - 4.2 μg kg⁻¹范围内可进行鉴定和确证。该方法适用于监管机构要求的鸡蛋中苏丹红染料残留的常规快速监测、筛查和确证。
