快速衍生-全自动固相萃取液质联用法测定食品中硝基呋喃代谢物
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摘要
目的建立食品中硝基呋喃代谢物快速衍生的全自动固相萃取-液质联用检测方法。方法采用混合标准溶液衍生后峰面积的响应值对衍生溶液、衍生剂用量、衍生温度和时间进行优化,以确定最佳衍生条件。衍生完成后,调节pH值至7.2±0.2,然后上全自动固相萃取仪,过HLB小柱净化。结果以5%三氯乙酸为衍生溶液,在60℃下,加入50μl快速衍生剂,4种硝基呋喃代谢物在10 min内可以完成衍生。经HLB小柱净化后,方法检出限达0.50μg/kg,加标回收率为86.7%～113.9%,RSD为2.0%～15.8%。结论快速衍生方法具有检测速度快、灵敏度低、前处理简单、回收率高等优点,能较好地满足食品中硝基呋喃代谢物检测的需求。
Objective To establish a testing method for the nitrofuran metabolites in foods by rapid derivatization and automatic solid phase extraction-liquid chromatography-mass spectrometry. Methods The response of peak area after derivatization with the mixed standard solution was optimized for derivatization solution, amount of derivatizing agent, derivatization temperature and time to derivatization. After derivatization was completed, pH was adjusted to 7.2±0.2, then purified by the HLB cartridge through the automatic solid phase extraction apparatus. Results With 5% trichloroacetic acid as the derivatization solution, 50 μl of the fast derivatizing agent was added and the temperature was set at 60 °C. The four kinds of nitrofuran metabolites were derivatized in 10 min. After purification by HLB cartridge, the detection limit of the method was 0.50 μg/kg and the recoveries range was 86.7%-113.9% and the RSD range was 2.0%-15.8%. Conclusion The rapid derivatization method had the advantages of fast detection speed, low sensitivity, simple pretreatment and high recovery rate, which can better meet the needs of nitrofuran metabolite detection in foods.
Objective To establish a testing method for the nitrofuran metabolites in foods by rapid derivatization and automatic solid phase extraction-liquid chromatography-mass spectrometry. Methods The response of peak area after derivatization with the mixed standard solution was optimized for derivatization solution, amount of derivatizing agent, derivatization temperature and time to derivatization. After derivatization was completed, pH was adjusted to 7.2±0.2, then purified by the HLB cartridge through the automatic solid phase extraction apparatus. Results With 5% trichloroacetic acid as the derivatization solution, 50 μl of the fast derivatizing agent was added and the temperature was set at 60 °C. The four kinds of nitrofuran metabolites were derivatized in 10 min. After purification by HLB cartridge, the detection limit of the method was 0.50 μg/kg and the recoveries range was 86.7%-113.9% and the RSD range was 2.0%-15.8%. Conclusion The rapid derivatization method had the advantages of fast detection speed, low sensitivity, simple pretreatment and high recovery rate, which can better meet the needs of nitrofuran metabolite detection in foods.
引文
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[10] 宋利军,于晖,程鑫,等.液相色谱-串联质谱法检测动物性食品中硝基呋喃代谢产物的残留[J].中国卫生检验杂志,2017,27(3):321-323.
[11] 华正罡,冯静,伊萍.超高效液相色谱-串联质谱法测定鸡肉中硝基呋喃类药物残留[J].中国卫生检验杂志,2014,24(11):1556-1559.
[12] 潘胜东,赵永纲,陈晓红,等.固相萃取-超快速液相色谱-串联质谱法测定鸡蛋中4种硝基呋喃代谢物残留[J].中国卫生检验杂志,2014,24(1):24-27.
[13] 王璟,杨楠,赵晶,等.液相色谱-串联质谱法检测水产品中硝基呋喃类代谢物[J].中国卫生检验杂志,2008,18(6):978-980.
[14] 尹怡,潘宇,刘书贵,等.超声辅助衍生-液相色谱/串联质谱法快速测定养殖水体中硝基呋喃类代谢物的残留量[J].分析试验室,2015,34(4):416-420.
[15] 尹怡,张宏峰,刘书贵,等.微波辅助衍生-液相色谱-串联质谱法快速测定养殖水体中5种硝基呋喃类代谢物残留[J].质谱学报,2016,37(2):106-113.
[2] 徐伟,耿士伟,刘路,等.硝基呋喃类药物及其代谢物检测方法的研究进展[J].天津农业科学,2018,24(8):16-20.
[3] 唐红梅,曾芳,李成洪.食品中硝基呋喃类药物及其代谢物残留检测的研究进展[J].食品安全质量检测学报,2016,7(10):3952-3959.
[4] 刘辉,梁德沛,花铁果,等.食品中硝基呋喃类药物及其代谢物残留检测技术的研究进展[J].食品安全质量检测学报,2013,4(2):383-388.
[5] 佘永新,李宝海,曹维强,等.动物性食品中硝基呋喃类药物及其代谢物残留检测技术的研究进展[J].现代科学仪器,2010(6):149-153.
[6] 彭鹏.硝基呋喃类兽药胶体金免疫层析检测方法研究[D].天津:天津科技大学,2016.
[7] 柳爱春,刘超,赵芸,等.免疫胶体金法快速检测水产品中硝基呋喃类代谢物的研究[J].浙江农业学报,2013,25(1):95-102.
[8] 辛少平,邓建朝,杨贤庆,等.高效液相色谱法测定硝基呋喃类药物代谢物及其在对虾体内的代谢[J].食品科学,2014,35(24):151-157.
[9] 高文惠,王姣姣,贾英民.分子印迹固相萃取-液相色谱法测定食品中硝基呋喃类药物残留[J].中国食品学报,2014,14(9):183-189.
[10] 宋利军,于晖,程鑫,等.液相色谱-串联质谱法检测动物性食品中硝基呋喃代谢产物的残留[J].中国卫生检验杂志,2017,27(3):321-323.
[11] 华正罡,冯静,伊萍.超高效液相色谱-串联质谱法测定鸡肉中硝基呋喃类药物残留[J].中国卫生检验杂志,2014,24(11):1556-1559.
[12] 潘胜东,赵永纲,陈晓红,等.固相萃取-超快速液相色谱-串联质谱法测定鸡蛋中4种硝基呋喃代谢物残留[J].中国卫生检验杂志,2014,24(1):24-27.
[13] 王璟,杨楠,赵晶,等.液相色谱-串联质谱法检测水产品中硝基呋喃类代谢物[J].中国卫生检验杂志,2008,18(6):978-980.
[14] 尹怡,潘宇,刘书贵,等.超声辅助衍生-液相色谱/串联质谱法快速测定养殖水体中硝基呋喃类代谢物的残留量[J].分析试验室,2015,34(4):416-420.
[15] 尹怡,张宏峰,刘书贵,等.微波辅助衍生-液相色谱-串联质谱法快速测定养殖水体中5种硝基呋喃类代谢物残留[J].质谱学报,2016,37(2):106-113.