复旦学报（医学版）
複旦學報（醫學版）
복단학보（의학판）
FUDAN UNIVERSITY JOURNAL OF MEDICAL SCIENCES
2010年
1期
68-70,87
,共4页
S-烯丙基-L-半胱氨酸%S-烯丙基-L-半胱氨酸亚砜%液质联用%大蒜提取物
S-烯丙基-L-半胱氨痠%S-烯丙基-L-半胱氨痠亞砜%液質聯用%大蒜提取物
S-희병기-L-반광안산%S-희병기-L-반광안산아풍%액질련용%대산제취물
S-allyl-L-cystein%S-allyl-L-cystein sulfoxide%liquid chromatography-mass spectrometry%extraction of garlic
目的 建立液质联用(liquid chromatography-mass spectrometry,LC-MS)定量分析测定大蒜提取物中S-烯丙基-L-半胱氨酸的方法.方法 采用LC-MS法检测,ZORBAX Eclipse XDB-C8(4.6 mm×250 mm,5 μm)色谱柱,流动相组成:1‰甲酸水-甲醇(95:5),流速:0.8 mL/min;柱后分流检测,分流比2:1;柱温:25 ℃;ESI电离源:负离子检测模式;干燥气流速:10.0 L/min;雾化室压力:30 psig;干燥气温度:350 ℃.选择离子方式检测(SIM):S-烯丙基-L-半胱氨酸m/z 160和S-烯丙基-L-半胱氨酸亚砜m/z 176.结果 S-烯丙基-L-半胱氨酸在0.062 5～2 μg/mL浓度范围内线性关系良好,检测限0.01 μg/mL,日内RSD 4.11%、日间RSD 4.49%, 方法平均回收率为101.63%.结论 此方法简单、准确,适于分析测定大蒜提取物中S-烯丙基-L-半胱氨酸的含量,并且测得该提取物中S-烯丙基-L-半胱氨酸的平均含量为0.514 μg/mg.
目的 建立液質聯用(liquid chromatography-mass spectrometry,LC-MS)定量分析測定大蒜提取物中S-烯丙基-L-半胱氨痠的方法.方法 採用LC-MS法檢測,ZORBAX Eclipse XDB-C8(4.6 mm×250 mm,5 μm)色譜柱,流動相組成:1‰甲痠水-甲醇(95:5),流速:0.8 mL/min;柱後分流檢測,分流比2:1;柱溫:25 ℃;ESI電離源:負離子檢測模式;榦燥氣流速:10.0 L/min;霧化室壓力:30 psig;榦燥氣溫度:350 ℃.選擇離子方式檢測(SIM):S-烯丙基-L-半胱氨痠m/z 160和S-烯丙基-L-半胱氨痠亞砜m/z 176.結果 S-烯丙基-L-半胱氨痠在0.062 5～2 μg/mL濃度範圍內線性關繫良好,檢測限0.01 μg/mL,日內RSD 4.11%、日間RSD 4.49%, 方法平均迴收率為101.63%.結論 此方法簡單、準確,適于分析測定大蒜提取物中S-烯丙基-L-半胱氨痠的含量,併且測得該提取物中S-烯丙基-L-半胱氨痠的平均含量為0.514 μg/mg.
목적 건립액질련용(liquid chromatography-mass spectrometry,LC-MS)정량분석측정대산제취물중S-희병기-L-반광안산적방법.방법 채용LC-MS법검측,ZORBAX Eclipse XDB-C8(4.6 mm×250 mm,5 μm)색보주,류동상조성:1‰갑산수-갑순(95:5),류속:0.8 mL/min;주후분류검측,분류비2:1;주온:25 ℃;ESI전리원:부리자검측모식;간조기류속:10.0 L/min;무화실압력:30 psig;간조기온도:350 ℃.선택리자방식검측(SIM):S-희병기-L-반광안산m/z 160화S-희병기-L-반광안산아풍m/z 176.결과 S-희병기-L-반광안산재0.062 5～2 μg/mL농도범위내선성관계량호,검측한0.01 μg/mL,일내RSD 4.11%、일간RSD 4.49%, 방법평균회수솔위101.63%.결론 차방법간단、준학,괄우분석측정대산제취물중S-희병기-L-반광안산적함량,병차측득해제취물중S-희병기-L-반광안산적평균함량위0.514 μg/mg.
Objective To develop a liquid chromatography-mass spectrometry (LC-MS) method for the determination of S-allyl-L-cystein in extraction of garlic. Methods A LC-MS method was established on a ZORBAX Eclipse XDB-C8(4.6 mm×250 mm, 5 μm)column with the mobile phase consisting of 1‰ formic acid water-methanol (95:5), flow rate of 0.8 mL/min and detection with post-column splitting. The split ratio was 2:1, column temperature was set at 25 ℃. The mass spectrometer equipped with ESI and the ion source was operated in negative mode. The dry gas flow was 10.0 L/min, the nebulizer pressure was 30 psig, and the vaporizer temperature was 350 ℃. SIM detector, S-allyl-L-cystein m/z 160 and S-allyl-L-cystein sulfoxide m/z 176. Results The calibration curves showed good linearity in the range of 0.062 5-2 μg/mL of S-allyl-L-cystein. The detection limit was 0.01 μg/mL. The within-day RSD was 4.11% and the day-to-day RSD was 4.49%.The average recovery for S-allyl-L-cystein was 101.63%. Conclusions The method is simple and accurate. It is adapted to determine and analyze S-allyl-L-cystein in extraction of garlic and the average content of S-allyl-L-cystein is 0.514 μg/mg.
