中国油脂
中國油脂
중국유지
CHINA OILS AND FATS
2015年
4期
90-93,94
,共5页
石金娥%王莹%王庆峰%刘桂华%王岩%侯宇
石金娥%王瑩%王慶峰%劉桂華%王巖%侯宇
석금아%왕형%왕경봉%류계화%왕암%후우
藻油%角鲨烯%GC-MS%含量%测定
藻油%角鯊烯%GC-MS%含量%測定
조유%각사희%GC-MS%함량%측정
algal oil%squalene%gas chromatography-mass spectrometry( GC-MS)%content%determi-nation
基于GB/T 22110—2008,建立一种利用GC-MS简单、快速测定藻油中角鲨烯含量的方法。考察了甲酯化试剂用量对甲酯化程度的影响与不同色谱柱对角鲨烯分离程度的影响。0.2 g藻油经1 mL 0.5 mol/L氢氧化钾-甲醇溶液进行甲酯化,正己烷提取后经HP-5 MS色谱柱分离,用GC-MS选择离子监测模式对角鲨烯进行定量测定。方法在10~500 mg/L范围内线性关系良好,相关系数r=0.9998,检出限为0.10 mg/L,加标回收率为92.14%~96.47%,此法也适用于其他植物油中角鲨烯含量的测定。通过比较“复合型”藻油和“非复合型”藻油样品成分及含量上的差异,得出两种类型的藻油除了脂肪酸含量存在差异外,“非复合型”藻油比“复合型”藻油角鲨烯含量高10倍多。
基于GB/T 22110—2008,建立一種利用GC-MS簡單、快速測定藻油中角鯊烯含量的方法。攷察瞭甲酯化試劑用量對甲酯化程度的影響與不同色譜柱對角鯊烯分離程度的影響。0.2 g藻油經1 mL 0.5 mol/L氫氧化鉀-甲醇溶液進行甲酯化,正己烷提取後經HP-5 MS色譜柱分離,用GC-MS選擇離子鑑測模式對角鯊烯進行定量測定。方法在10~500 mg/L範圍內線性關繫良好,相關繫數r=0.9998,檢齣限為0.10 mg/L,加標迴收率為92.14%~96.47%,此法也適用于其他植物油中角鯊烯含量的測定。通過比較“複閤型”藻油和“非複閤型”藻油樣品成分及含量上的差異,得齣兩種類型的藻油除瞭脂肪痠含量存在差異外,“非複閤型”藻油比“複閤型”藻油角鯊烯含量高10倍多。
기우GB/T 22110—2008,건립일충이용GC-MS간단、쾌속측정조유중각사희함량적방법。고찰료갑지화시제용량대갑지화정도적영향여불동색보주대각사희분리정도적영향。0.2 g조유경1 mL 0.5 mol/L경양화갑-갑순용액진행갑지화,정기완제취후경HP-5 MS색보주분리,용GC-MS선택리자감측모식대각사희진행정량측정。방법재10~500 mg/L범위내선성관계량호,상관계수r=0.9998,검출한위0.10 mg/L,가표회수솔위92.14%~96.47%,차법야괄용우기타식물유중각사희함량적측정。통과비교“복합형”조유화“비복합형”조유양품성분급함량상적차이,득출량충류형적조유제료지방산함량존재차이외,“비복합형”조유비“복합형”조유각사희함량고10배다。
Based on GB/T 22110—2008 , a simple and rapid method for the determination of squalene in algal oil by gas chromatography-mass spectrometry(GC -MS) was developed. The effect of dosage of methyl esterification reagent on the degree of esterification was investigated, and the impact of different chromatographic columns on separation degree of squalene was also studied. After 0. 2 g algal oil was methyl esterified by 1 mL of 0 . 5 mol/L potassium hydroxide-methanol solution and extracted by hex-ane, it was separated by HP-5MS chromatographic column, then the squalene was determined quantita-tively by GC-MS in selected ion monitoring mode. The linear range, the relative coefficient, the limit of detection and the recovery of standard addition of the method were 10-500 mg/L, 0. 999 8, 0. 10 mg/L, 92. 14% -96. 47%, respectively. The method also could be applied to other vegetable oils. By compa-ring the difference between“complex” and“non-complex” algal oils in composition and content, it was found that in addition to the different contents of fatty acid in these two types of algal oils, the content of squalene in “non-complex” algal oil was 10 times higher than “complex” algal oil.