海峡药学
海峽藥學
해협약학
Strait Pharmaceutical Journal
2015年
10期
36-39
,共4页
UPLC-QTOF-MS%性激素%化妆品%非法添加%快速测定
UPLC-QTOF-MS%性激素%化妝品%非法添加%快速測定
UPLC-QTOF-MS%성격소%화장품%비법첨가%쾌속측정
UPLC-QTOF-MS%Sexhormone%Cosmetics%Illegally add%Rapid and accurate
目的 建立快速、准确检测化妆品中非法添加的7 种性激素的方法 . 方法 采用 UPLC-QTOF-MS法,使用 Agilent ZORBAX Extend-C18 (2.1 ×50mm,1.8μm)柱,以乙腈(A)水(B)为流动相,流速0.3mL· min -1,柱温:30℃;选择ESI离子源,正负离子扫描等模式测定7 种性激素.通过比较各样品峰与对照品峰的分子离子峰、二级碎片离子峰、色谱保留时间等信息确定添加的成分,并根据外标法以质谱峰面积计算添加成分的含量. 结果 在上述色谱及质谱条件下,雌三醇、雌二醇、雌酮、己烯雌酚、睾丸酮、甲睾酮、黄体酮7 种性激素能被准确检出,最低检出限(LOD)均在3~80ng· mg -1之间,标准加样回收率均在80.3%~103.5%之间. 结论 本方法 快速准确方便、灵敏度较高,可作为化妆品中非法添加性激素的测定方法 .
目的 建立快速、準確檢測化妝品中非法添加的7 種性激素的方法 . 方法 採用 UPLC-QTOF-MS法,使用 Agilent ZORBAX Extend-C18 (2.1 ×50mm,1.8μm)柱,以乙腈(A)水(B)為流動相,流速0.3mL· min -1,柱溫:30℃;選擇ESI離子源,正負離子掃描等模式測定7 種性激素.通過比較各樣品峰與對照品峰的分子離子峰、二級碎片離子峰、色譜保留時間等信息確定添加的成分,併根據外標法以質譜峰麵積計算添加成分的含量. 結果 在上述色譜及質譜條件下,雌三醇、雌二醇、雌酮、己烯雌酚、睪汍酮、甲睪酮、黃體酮7 種性激素能被準確檢齣,最低檢齣限(LOD)均在3~80ng· mg -1之間,標準加樣迴收率均在80.3%~103.5%之間. 結論 本方法 快速準確方便、靈敏度較高,可作為化妝品中非法添加性激素的測定方法 .
목적 건립쾌속、준학검측화장품중비법첨가적7 충성격소적방법 . 방법 채용 UPLC-QTOF-MS법,사용 Agilent ZORBAX Extend-C18 (2.1 ×50mm,1.8μm)주,이을정(A)수(B)위류동상,류속0.3mL· min -1,주온:30℃;선택ESI리자원,정부리자소묘등모식측정7 충성격소.통과비교각양품봉여대조품봉적분자리자봉、이급쇄편리자봉、색보보류시간등신식학정첨가적성분,병근거외표법이질보봉면적계산첨가성분적함량. 결과 재상술색보급질보조건하,자삼순、자이순、자동、기희자분、고환동、갑고동、황체동7 충성격소능피준학검출,최저검출한(LOD)균재3~80ng· mg -1지간,표준가양회수솔균재80.3%~103.5%지간. 결론 본방법 쾌속준학방편、령민도교고,가작위화장품중비법첨가성격소적측정방법 .
OBJECTIVE To establish a rapid,accurate method for determination of 7 sexhormone,which were illegally added to cosmetics.METHODS The UPLC-QTOF-MS method was adopted.The analytes were separated on a Agilent ZORBAX Extend-C18(2.1 ×50mm,1.8μm)with acetonitrile(A)and water(B)and the flow rate of 0.3mL· min-1 ,and the column temperature was 30℃.A positive and negative ions( ESI) source was used to sepa-rate and quantitatively determinate 7 sexhormones.The obtained molecular ions,fragment ions and retention time were used to identify the 7 sexhormones by comparison with those of refarate substances.The obtained peak areas were used to determinate the accurate content of anti-diabetic drugs in cosmetics according to the external standard meth-od.RESULTS 7sexhormonesincludingestriol,estradiol,estrone,diethylstilbestrol,testosterone,methyltestosterone and progesterone were obtained under this UPLC and QTOF-MS condition.The detection limit were in the range of 4~80ng· mg -1 and the standard addition recoveries were in the range of 80.3%~103.5%.CONCLUSION The method is rapid,accurate and conveniency,which can be used for the determination of illegal added sexhormones in cosmetics.
