食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2014年
9期
2729-2735
,共7页
酪胺%分子印迹固相萃取%高效液相色谱法%酱油
酪胺%分子印跡固相萃取%高效液相色譜法%醬油
락알%분자인적고상췌취%고효액상색보법%장유
tyramine%molecularly imprinted solid phase extraction%high performance liquid chromatography%soy sauce
目的:建立分子印迹固相萃取与高效液相色谱联用快速测定酱油中酪胺含量的方法。方法采用本体聚合法以酪胺为模板分子,对乙烯基苯甲酸(P-VBA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)为交联剂,制备分子印迹聚合物为填料自制固相萃取柱。对上样溶剂、流速、淋洗及洗脱溶剂等条件进行优化,采用优化的条件萃取酱油中的酪胺,高效液相色谱测定。结果固相萃取优化条件为:上样溶剂为5%乙醇水溶液,10%甲醇为淋洗液,40%乙腈为洗脱液,流速均控制在0.5 mL/min。在加标浓度为5μg/mL 和10μg/mL的3种酱油所得到的平均回收率在86.95%~106.06%之间。结论本方法能快速分离酱油中酪胺,样品前处理效率高,方法灵敏度高,适用于食品中酪胺的痕量分析。
目的:建立分子印跡固相萃取與高效液相色譜聯用快速測定醬油中酪胺含量的方法。方法採用本體聚閤法以酪胺為模闆分子,對乙烯基苯甲痠(P-VBA)為功能單體,乙二醇二甲基丙烯痠酯(EGDMA)為交聯劑,製備分子印跡聚閤物為填料自製固相萃取柱。對上樣溶劑、流速、淋洗及洗脫溶劑等條件進行優化,採用優化的條件萃取醬油中的酪胺,高效液相色譜測定。結果固相萃取優化條件為:上樣溶劑為5%乙醇水溶液,10%甲醇為淋洗液,40%乙腈為洗脫液,流速均控製在0.5 mL/min。在加標濃度為5μg/mL 和10μg/mL的3種醬油所得到的平均迴收率在86.95%~106.06%之間。結論本方法能快速分離醬油中酪胺,樣品前處理效率高,方法靈敏度高,適用于食品中酪胺的痕量分析。
목적:건립분자인적고상췌취여고효액상색보련용쾌속측정장유중락알함량적방법。방법채용본체취합법이락알위모판분자,대을희기분갑산(P-VBA)위공능단체,을이순이갑기병희산지(EGDMA)위교련제,제비분자인적취합물위전료자제고상췌취주。대상양용제、류속、림세급세탈용제등조건진행우화,채용우화적조건췌취장유중적락알,고효액상색보측정。결과고상췌취우화조건위:상양용제위5%을순수용액,10%갑순위림세액,40%을정위세탈액,류속균공제재0.5 mL/min。재가표농도위5μg/mL 화10μg/mL적3충장유소득도적평균회수솔재86.95%~106.06%지간。결론본방법능쾌속분리장유중락알,양품전처리효솔고,방법령민도고,괄용우식품중락알적흔량분석。
Objective To establish a method for determination of tyramine in soy sauce by molecular imprinting solid phase extraction (MISPE) and high performance liquid chromatography (HPLC). Methods Tyramine molecular imprinted polymer (MIP) was prepared by bulk polymerization using tyramine, p-vinylbenzoic acid and ethylene glycol dimethacrylate as template, functional monomer and cross-linker, respectively. The MISPE column was made using MIP as filler. The extraction conditions were optimized before HPLC determination. Results The optimized conditions were as follows:the loading, washing, eluting solvent were 5% ethanol, 10% methanol and 40% acetonitrile, respectively, and the flow velocity was 0.5 mL/min. The recoveries were in the range of 86.95%~106.06% at the spiked level of 5 μg/mL and 10μg/mL. Conclusion The proposed method allows the efficient extraction of tyramine in soy sauce in pre-treatment and with high sensitivity, which can be applied to trace analysis of tyramine in food.