分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
9期
1329-1334
,共6页
曹玉嫔%闫丽珍%黄红丽%邓必阳
曹玉嬪%閆麗珍%黃紅麗%鄧必暘
조옥빈%염려진%황홍려%산필양
硒%高效液相色谱-电感耦合等离子体质谱%牛蒡%三七%超声提取
硒%高效液相色譜-電感耦閤等離子體質譜%牛蒡%三七%超聲提取
서%고효액상색보-전감우합등리자체질보%우방%삼칠%초성제취
Selenium%High performance liquid chromatography-inductively coupled plasma mass spectrometry%Burdock%Panax notoginseng%Ultrasonic extraction
用蛋白酶K和脂肪酶作为提取剂、用超声波辅助提取牛蒡和三七样品中的硒形态。建立了高效液相色谱-电感耦合等离子体质谱联用技术测定牛蒡和三七样品中硒代胱氨酸( SeCys2)、亚硒酸盐[ SeⅣ]、硒代蛋氨酸(SeMet)和硒酸盐[SeⅥ]的新方法。用8 mmol/L pH 5.0的柠檬酸作为流动相,在8 min内可分离4种硒形态。利用CH4作为DRC反应气体,可消除了40 Ar40 Ar+对80 Se+的干扰,提高了准确度。 SeCys2、SeⅣ、SeMet和SeⅥ的检出限分别为0.088,0.033,0.30和0.17 ng/mL,相关系数(R2)均大于0.9995,加标回收率范围为95.1%~114.6%,RSD<3%。将本方法应用于牛蒡和三七中硒形态分析,结果令人满意。
用蛋白酶K和脂肪酶作為提取劑、用超聲波輔助提取牛蒡和三七樣品中的硒形態。建立瞭高效液相色譜-電感耦閤等離子體質譜聯用技術測定牛蒡和三七樣品中硒代胱氨痠( SeCys2)、亞硒痠鹽[ SeⅣ]、硒代蛋氨痠(SeMet)和硒痠鹽[SeⅥ]的新方法。用8 mmol/L pH 5.0的檸檬痠作為流動相,在8 min內可分離4種硒形態。利用CH4作為DRC反應氣體,可消除瞭40 Ar40 Ar+對80 Se+的榦擾,提高瞭準確度。 SeCys2、SeⅣ、SeMet和SeⅥ的檢齣限分彆為0.088,0.033,0.30和0.17 ng/mL,相關繫數(R2)均大于0.9995,加標迴收率範圍為95.1%~114.6%,RSD<3%。將本方法應用于牛蒡和三七中硒形態分析,結果令人滿意。
용단백매K화지방매작위제취제、용초성파보조제취우방화삼칠양품중적서형태。건립료고효액상색보-전감우합등리자체질보련용기술측정우방화삼칠양품중서대광안산( SeCys2)、아서산염[ SeⅣ]、서대단안산(SeMet)화서산염[SeⅥ]적신방법。용8 mmol/L pH 5.0적저몽산작위류동상,재8 min내가분리4충서형태。이용CH4작위DRC반응기체,가소제료40 Ar40 Ar+대80 Se+적간우,제고료준학도。 SeCys2、SeⅣ、SeMet화SeⅥ적검출한분별위0.088,0.033,0.30화0.17 ng/mL,상관계수(R2)균대우0.9995,가표회수솔범위위95.1%~114.6%,RSD<3%。장본방법응용우우방화삼칠중서형태분석,결과령인만의。
A high performance liquid chromatography-inductively coupled plasma mass spectrometric ( HPLC-ICP-MS) method for analysis of selenocystine (SeCys2), selenite (SeⅣ), selenomethionine (SeMet) and selenate ( SeⅥ) was described. Chromatographic separation was performed using 8 mmol/L citric acid solution (pH 5). The potentially interfering 40Ar40Ar+ at selenium masses of m/z 80 was reduced using CH4 as a reactive cell gas in the dynamic reaction cell. The selenium species was extracted using ultrasonic extraction system with a mixture of protease K and lipase. The limits of detection for SeCys2 , SeⅣ, SeMet, and SeⅥwere observed as 0. 088, 0. 033, 0. 30, and 0. 17 ng/mL, respectively. The correlation coefficients were greater than 0 . 9995 . The recoveries were observed in the range of 95 . 1%-114 . 6%. The developed method was successfully applied for the determination of selenium species in Burdock and Panax notoginseng.