河北省科学院学报
河北省科學院學報
하북성과학원학보
JOURNAL OF THE HEBEI ACADEMY OF SCIENCES
2014年
4期
66-74
,共9页
李强%夏静%吴春敏%张岩
李彊%夏靜%吳春敏%張巖
리강%하정%오춘민%장암
高分辨质谱%保健品%降糖药物%快筛
高分辨質譜%保健品%降糖藥物%快篩
고분변질보%보건품%강당약물%쾌사
High performance liquid chromatography-ion trap-time of flight tandem mass spec-trometry(HPLC-IT-TOF-MS)%Health foods%Antidiabetic drugs%Screening
采用高效液相色谱-离子阱飞行时间串联高分辨质谱对于保健品中降糖类药物共11种成分进行快速筛查、定性识别和准确定量。样品经含甲醇溶液超声提取,提取液经QuEChERS吸附剂净化,以C18色谱柱(150mm ×2.0mm ,3.0μm )分离,5mmol/L乙酸铵溶液和0.5%甲酸乙腈为流动相梯度洗脱,正离子模式扫描。结果表明,11种化合物在2~1000μg/L范围内呈良好的线性相关性,相关系数均大于0.991。保健品样品中各化合物的定量限(以信噪比≥10计)分别为2.0~50μg/kg。在低、中、高3个添加水平下,各化合物的平均回收率为72.3%~118.1%,相对标准偏差(RSD )为0.5%~8.4%。该方法利用精确质量数匹配和自建标准谱库检索,实现快速筛查,并使用多级特征碎片离子进行确证,具有简便、快速、高效、准确等优点,适用于保健食品中降压降糖类药物的快速筛查和测定。
採用高效液相色譜-離子阱飛行時間串聯高分辨質譜對于保健品中降糖類藥物共11種成分進行快速篩查、定性識彆和準確定量。樣品經含甲醇溶液超聲提取,提取液經QuEChERS吸附劑淨化,以C18色譜柱(150mm ×2.0mm ,3.0μm )分離,5mmol/L乙痠銨溶液和0.5%甲痠乙腈為流動相梯度洗脫,正離子模式掃描。結果錶明,11種化閤物在2~1000μg/L範圍內呈良好的線性相關性,相關繫數均大于0.991。保健品樣品中各化閤物的定量限(以信譟比≥10計)分彆為2.0~50μg/kg。在低、中、高3箇添加水平下,各化閤物的平均迴收率為72.3%~118.1%,相對標準偏差(RSD )為0.5%~8.4%。該方法利用精確質量數匹配和自建標準譜庫檢索,實現快速篩查,併使用多級特徵碎片離子進行確證,具有簡便、快速、高效、準確等優點,適用于保健食品中降壓降糖類藥物的快速篩查和測定。
채용고효액상색보-리자정비행시간천련고분변질보대우보건품중강당류약물공11충성분진행쾌속사사、정성식별화준학정량。양품경함갑순용액초성제취,제취액경QuEChERS흡부제정화,이C18색보주(150mm ×2.0mm ,3.0μm )분리,5mmol/L을산안용액화0.5%갑산을정위류동상제도세탈,정리자모식소묘。결과표명,11충화합물재2~1000μg/L범위내정량호적선성상관성,상관계수균대우0.991。보건품양품중각화합물적정량한(이신조비≥10계)분별위2.0~50μg/kg。재저、중、고3개첨가수평하,각화합물적평균회수솔위72.3%~118.1%,상대표준편차(RSD )위0.5%~8.4%。해방법이용정학질량수필배화자건표준보고검색,실현쾌속사사,병사용다급특정쇄편리자진행학증,구유간편、쾌속、고효、준학등우점,괄용우보건식품중강압강당류약물적쾌속사사화측정。
A method w as developed for the screening and confirmation and quantification of 11 antidiabetic drugs in healthy foods by high performance liquid chromatography ion trap time of flight tandem mass spectrometry (HPLC‐IT‐TOF‐MS) .The analytes in the sample were ex‐tracted with methanol and the extract was purified with the mixed QuEChERS sorbents .In the chromatographic analysis ,the 11 antidiabetic drugs were separated on a C18 column with the gradient elution using the mobile phases of acetonitrile and water containing 0 .5% acetic acid .The mass analyzer was performed in positive modes in one injection .The results showed that the line arranges of the 11 compounds were 2-1000μg/L with the correlation coefficients above 0 .991 and the limits of quantification(LOQ ,S/N≥10)were2 .0-50 .0μg/kg for capsule <br> and oral solution ,respectively .T he method validation w as carried out at three spiked levels , and the recoveries were 72 .3% -118 .1% with the relative standard deviations (RSDs) of 0 .5% -8 .4% .The screening of analytes was performed by precision mass matching and li‐brary searching .These condary fragmention spectra were employed to the confirmation .This method is simple ,fast ,reliable ,and can be applied to the simultaneous screening and determi‐nation of hormones in health foods .