酿酒科技
釀酒科技
양주과기
LIQUOR-MAKING SCIENCE & TECHNOLOGY
2014年
9期
100-103
,共4页
邵秋荣%刘斌%石金娥%孟昭建%方邢有%丁晓%李天宝
邵鞦榮%劉斌%石金娥%孟昭建%方邢有%丁曉%李天寶
소추영%류빈%석금아%맹소건%방형유%정효%리천보
邻苯二甲酸酯%超高效液相-质谱法%白酒%红酒%洋酒
鄰苯二甲痠酯%超高效液相-質譜法%白酒%紅酒%洋酒
린분이갑산지%초고효액상-질보법%백주%홍주%양주
phthalate esters%UPLC-MS%Baijiu(liquor)%red wine%imported wine
建立了液相色谱质谱联用法同时测定酒中污染物23种邻苯二甲酸酯类增塑剂残留量的检测方法。样品经过沸水加热除去乙醇后,正己烷提取,经Waters ACQUITY UPLC? BEH C18色谱柱分离,以甲醇和0.1%甲酸溶液为流动相梯度洗脱,电喷雾正离子模式离子化,选择反应监测方式监测,串联质谱测定,外标法定量。结果显示,各目标物在0.1~10.0 mg/L浓度范围内的线性关系良好,相关系数大于0.993。该方法对酒中23种邻苯二甲酸酯化合物的定量限为0.1 mg/kg,23种邻苯酸二甲酸酯的回收率为87%~102%。结果表明,该方法简便快速、灵敏可靠、经济有效,适用于酒中污染物邻苯二甲酸酯检测的需要。
建立瞭液相色譜質譜聯用法同時測定酒中汙染物23種鄰苯二甲痠酯類增塑劑殘留量的檢測方法。樣品經過沸水加熱除去乙醇後,正己烷提取,經Waters ACQUITY UPLC? BEH C18色譜柱分離,以甲醇和0.1%甲痠溶液為流動相梯度洗脫,電噴霧正離子模式離子化,選擇反應鑑測方式鑑測,串聯質譜測定,外標法定量。結果顯示,各目標物在0.1~10.0 mg/L濃度範圍內的線性關繫良好,相關繫數大于0.993。該方法對酒中23種鄰苯二甲痠酯化閤物的定量限為0.1 mg/kg,23種鄰苯痠二甲痠酯的迴收率為87%~102%。結果錶明,該方法簡便快速、靈敏可靠、經濟有效,適用于酒中汙染物鄰苯二甲痠酯檢測的需要。
건립료액상색보질보련용법동시측정주중오염물23충린분이갑산지류증소제잔류량적검측방법。양품경과비수가열제거을순후,정기완제취,경Waters ACQUITY UPLC? BEH C18색보주분리,이갑순화0.1%갑산용액위류동상제도세탈,전분무정리자모식리자화,선택반응감측방식감측,천련질보측정,외표법정량。결과현시,각목표물재0.1~10.0 mg/L농도범위내적선성관계량호,상관계수대우0.993。해방법대주중23충린분이갑산지화합물적정량한위0.1 mg/kg,23충린분산이갑산지적회수솔위87%~102%。결과표명,해방법간편쾌속、령민가고、경제유효,괄용우주중오염물린분이갑산지검측적수요。
The residual quantity of 23 kinds of p hthalate esters in liquor was measured simultaneously by UPLC-MS. Firstly, liquor sample was heated by boiling water to remove ethanol, then extracted with n-hexane, and then isolated by centrifugation, the separation was perfomed on a Waters ACQUITY UPLC? BEH C18 column with aradient elution using methanol and 0.1%formic acid, and the electrospray ionization (ESI) source in positive ion mode was used for multiple reaction monitoring (RSM), then tandem MS was used for the measurement, and the external standard method was used for the quantification.The measurement results suggested that, the linear relationship of each phthalate ester was good within the range between 0.1~10.0 mg/kg and the correlation coefficient was above 0.993. The detection limits of such method were 0.1~0.5 mg/kg. The recoveries of 23 kinds of phthalate esters were ranged from 87.5%~101.2%with the relative standard deviations of 1.7%~5.8%. Such method was easy,fast,sensitive,and suitable for the determination of 23 kinds of phalate esters in liquor samples.