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
1期
70-76
,共7页
章骞%郑福来%翁凌%张凌晶%曹敏杰
章鶱%鄭福來%翁凌%張凌晶%曹敏傑
장건%정복래%옹릉%장릉정%조민걸
鲍鱼内脏%牛磺酸%提取%检测
鮑魚內髒%牛磺痠%提取%檢測
포어내장%우광산%제취%검측
abalone viscera%taurine%extraction%determination
目的:以皱纹盘鲍内脏为原料,优化高纯度牛磺酸的提取工艺,并建立用高压液相色谱检测牛磺酸纯度的方法。方法经水煮、乙醇抽提、蒸发浓缩、沉淀、活性炭处理、结晶等步骤,获得高纯度天然牛磺酸。用高压液相色谱检测牛磺酸纯度的方法为:色谱柱:Discovery C18;流动相:甲醇-0.05 mol/L乙酸钠缓冲液(pH 5.3)(v/v,50:50);流速:1 mL/min;检测波长:330 nm;柱温:室温。结果该提取工艺能从1 kg 鲍鱼内脏中提取得到天然牛磺酸3.07 g。采用该检测方法,牛磺酸的出峰时间为6.037 min,在1~20μg/mL浓度范围内线性关系良好(R2=0.9999),最低检出限为0.03μg/mL,最低定量限为0.12μg/mL,样品测定的平均回收率为99.44%(RSD=0.25%),方法的精密度和稳定性好(RSD<1%),用该方法检测提取得到的牛磺酸纯度为96.06%。采用红外光谱法(IR)对提取得到的鲍鱼内脏牛磺酸进一步作结构鉴定,发现它与标准品的红外特征吸收峰一致。结论获得了高纯度牛磺酸的提取工艺。本方法精密度和稳定性好,回收率高。
目的:以皺紋盤鮑內髒為原料,優化高純度牛磺痠的提取工藝,併建立用高壓液相色譜檢測牛磺痠純度的方法。方法經水煮、乙醇抽提、蒸髮濃縮、沉澱、活性炭處理、結晶等步驟,穫得高純度天然牛磺痠。用高壓液相色譜檢測牛磺痠純度的方法為:色譜柱:Discovery C18;流動相:甲醇-0.05 mol/L乙痠鈉緩遲液(pH 5.3)(v/v,50:50);流速:1 mL/min;檢測波長:330 nm;柱溫:室溫。結果該提取工藝能從1 kg 鮑魚內髒中提取得到天然牛磺痠3.07 g。採用該檢測方法,牛磺痠的齣峰時間為6.037 min,在1~20μg/mL濃度範圍內線性關繫良好(R2=0.9999),最低檢齣限為0.03μg/mL,最低定量限為0.12μg/mL,樣品測定的平均迴收率為99.44%(RSD=0.25%),方法的精密度和穩定性好(RSD<1%),用該方法檢測提取得到的牛磺痠純度為96.06%。採用紅外光譜法(IR)對提取得到的鮑魚內髒牛磺痠進一步作結構鑒定,髮現它與標準品的紅外特徵吸收峰一緻。結論穫得瞭高純度牛磺痠的提取工藝。本方法精密度和穩定性好,迴收率高。
목적:이추문반포내장위원료,우화고순도우광산적제취공예,병건립용고압액상색보검측우광산순도적방법。방법경수자、을순추제、증발농축、침정、활성탄처리、결정등보취,획득고순도천연우광산。용고압액상색보검측우광산순도적방법위:색보주:Discovery C18;류동상:갑순-0.05 mol/L을산납완충액(pH 5.3)(v/v,50:50);류속:1 mL/min;검측파장:330 nm;주온:실온。결과해제취공예능종1 kg 포어내장중제취득도천연우광산3.07 g。채용해검측방법,우광산적출봉시간위6.037 min,재1~20μg/mL농도범위내선성관계량호(R2=0.9999),최저검출한위0.03μg/mL,최저정량한위0.12μg/mL,양품측정적평균회수솔위99.44%(RSD=0.25%),방법적정밀도화은정성호(RSD<1%),용해방법검측제취득도적우광산순도위96.06%。채용홍외광보법(IR)대제취득도적포어내장우광산진일보작결구감정,발현타여표준품적홍외특정흡수봉일치。결론획득료고순도우광산적제취공예。본방법정밀도화은정성호,회수솔고。
Objective The viscera from abalone (Haliotis discus hannai) was used as raw materials to isolate natural taurine and an HPLC method for the determination of the purity of taurine was established. Methods Natural taurine was isolated by combining methods of high temperature stewing, activated carbon treatment, ethanol extraction, concentration, precipitation and crystallization. The HPLC method for determination of the purity of taurine was performed on a Discovery C18 column eluted with a mobile phase of 50% methyl alcohol and 50% sodium acetate (pH 5.3) at flow rate of 1.0 mL/min at room tem-perature and detected by a UV detector at 330 nm. Results Taurine (3.07 g) was isolated from 1 kg ab-alone viscera by the extraction method. The retention time of taurine was at 6.037 min on HPLC and the method showed a good linearity within concentration of 1~20 μg/mL with R2 of 0.9999. The detection limit was 0.03 μg/mL and the quantitative detection limit was 0.12 μg/mL with an average recovery of sample of 99.44% (RSD=0.25%). The precision and stability of this method was optimal (RSD<1%). Us-ing this method, the purity of taurine extracted from abalone viscera reached 96.06%. The structure of the obtained taurine was further analyzed by infrared spectrometer and its characteristic absorption peak was consistent with that of the standard taurine. Conclusion The extraction method of taurine with high pur-ity was established. The determination method resulted in optimal precision and stability as well as a high recovery of sample.