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
7期
2059-2065
,共7页
黄焘%陶保华%陈启%任一平
黃燾%陶保華%陳啟%任一平
황도%도보화%진계%임일평
胆碱%L-肉碱%乙酰基-L-肉碱%牛磺酸%人乳
膽堿%L-肉堿%乙酰基-L-肉堿%牛磺痠%人乳
담감%L-육감%을선기-L-육감%우광산%인유
choline%L-carnitine%acetyl-L-Carnitine%taurine%human milk
目的：建立一种简单、快速、灵敏的可以同时测定人乳中胆碱、L-肉碱、乙酰基-L-肉碱和牛磺酸的超高效液相色谱-串联质谱法。方法样品经甲醇沉淀蛋白、乙醚去除非极性杂质, UPLC BEH Amide色谱柱分离后采用保留时间和多反应离子检测(MRM)定性、定量,同位素内标校正。结果牛磺酸的定量下限(LOQ)为0.02 mg/100 g,胆碱、L-肉碱和乙酰基-L-肉碱的LOQ均为0.003 mg/100 g。标准加入法测定所有被测物的高、中、低三个浓度加标水平的回收率在84.8%~90.3%之间,相对标准偏差(RSD)在1.7%~5.3%之间。4种被测物在各自浓度范围内线性良好, R2均大于0.999。结论本文建立了同时测定人乳中胆碱、L-肉碱、乙酰基-L-肉碱和牛磺酸的超高效液相色谱-串联质谱法。方法前处理简单、快速,样品需要量少；采用质谱检测器同位素内标一对一校正定量,检测结果准确、灵敏。方法可以为人乳中相关营养素含量的调查、研究和为配方奶粉人乳化提供技术支持。
目的：建立一種簡單、快速、靈敏的可以同時測定人乳中膽堿、L-肉堿、乙酰基-L-肉堿和牛磺痠的超高效液相色譜-串聯質譜法。方法樣品經甲醇沉澱蛋白、乙醚去除非極性雜質, UPLC BEH Amide色譜柱分離後採用保留時間和多反應離子檢測(MRM)定性、定量,同位素內標校正。結果牛磺痠的定量下限(LOQ)為0.02 mg/100 g,膽堿、L-肉堿和乙酰基-L-肉堿的LOQ均為0.003 mg/100 g。標準加入法測定所有被測物的高、中、低三箇濃度加標水平的迴收率在84.8%~90.3%之間,相對標準偏差(RSD)在1.7%~5.3%之間。4種被測物在各自濃度範圍內線性良好, R2均大于0.999。結論本文建立瞭同時測定人乳中膽堿、L-肉堿、乙酰基-L-肉堿和牛磺痠的超高效液相色譜-串聯質譜法。方法前處理簡單、快速,樣品需要量少；採用質譜檢測器同位素內標一對一校正定量,檢測結果準確、靈敏。方法可以為人乳中相關營養素含量的調查、研究和為配方奶粉人乳化提供技術支持。
목적：건립일충간단、쾌속、령민적가이동시측정인유중담감、L-육감、을선기-L-육감화우광산적초고효액상색보-천련질보법。방법양품경갑순침정단백、을미거제비겁성잡질, UPLC BEH Amide색보주분리후채용보류시간화다반응리자검측(MRM)정성、정량,동위소내표교정。결과우광산적정량하한(LOQ)위0.02 mg/100 g,담감、L-육감화을선기-L-육감적LOQ균위0.003 mg/100 g。표준가입법측정소유피측물적고、중、저삼개농도가표수평적회수솔재84.8%~90.3%지간,상대표준편차(RSD)재1.7%~5.3%지간。4충피측물재각자농도범위내선성량호, R2균대우0.999。결론본문건립료동시측정인유중담감、L-육감、을선기-L-육감화우광산적초고효액상색보-천련질보법。방법전처리간단、쾌속,양품수요량소；채용질보검측기동위소내표일대일교정정량,검측결과준학、령민。방법가이위인유중상관영양소함량적조사、연구화위배방내분인유화제공기술지지。
Objective To establish a rapid and sensitive method which can determine choline, L-carnitine, acetyl-L-carnitine and taurine in human milk by ultra-performance liquid-chromatography tandem mass spec-trometry (UPLC-MS/MS). Methods The non-polar substances and protein were removed from samples by ether and methanol respectively. The sample extracts were separated by a UPLC BEH Amide column. The de-tection was performed with mass spectrometry under multiple reaction monitoring (MRM) mode with stable isotopedilution method. Results LOQs of choline, L-carnitine, acetyl-L-carnitine and taurine were between 0.003 mg/100 g and 0.02 mg/100 g. The spiked recoveries were 84.8%~90.3%. The precision RSD were below 5.3%. The lineal range was with high correlation coefficients (R2>0.999). Conclusion A simultaneous quanti-fication of choline, L-carnitine, acetyl-L-carnitine and taurine in human milk was developed by using a UHPLC-MS/MS method. The sample preparation was simple, rapid and required small volume of samples. Four stable isotope standards which provide high precision and accurate were used for each analyte. The de-veloped method was suitable for the study of four kinds of analytes which were concentrated in human milk and provided the technical support for the infant formula.
