色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
6期
566-572
,共7页
黄娟%殷耀%徐锦忠%刘艳%陈国松%张晓燕%杨雯筌%沈崇钰%陈惠兰%张睿
黃娟%慇耀%徐錦忠%劉豔%陳國鬆%張曉燕%楊雯筌%瀋崇鈺%陳惠蘭%張睿
황연%은요%서금충%류염%진국송%장효연%양문전%침숭옥%진혜란%장예
固相萃取%高效液相色谱-串联质谱%链霉素%双氢链霉素%花粉
固相萃取%高效液相色譜-串聯質譜%鏈黴素%雙氫鏈黴素%花粉
고상췌취%고효액상색보-천련질보%련매소%쌍경련매소%화분
solid phase extraction( SPE)%high performance liquid chromatography-tandem mass spectrometry(HPLC-MS / MS)%streptomycin%dihydrostreptomycin%pollens
建立了花粉中链霉素（ streptomycin，STR）与双氢链霉素（ dihydrostreptomycin，DHS）的高效液相色谱-串联质谱（HPLC-MS / MS）检测方法。样品经提取液提取、三氯甲烷沉淀蛋白后，用 C18固相萃取柱进行富集净化，采用 HPLC-MS / MS 对目标物进行定性确证和定量分析。在 Protemix WCX-NP5色谱柱（100 mm ×2.1 mm，5μm）上以5％（v / v）甲酸、20 mmol / L 醋酸铵和甲醇为流动相进行梯度洗脱分离；质谱采集模式为电喷雾正离子监测模式。链霉素和双氢链霉素的检出限（以信噪比（ S / N）＝3计）均为5μg / kg，定量限（以 S / N ＝10计）均为10μg / kg；在10~200μg / L 的质量浓度范围内呈现良好的线性关系，相关系数（ r）大于0.99。本底空白的松花粉、玉米花粉、茶花粉、葵花粉、油菜花粉、杂花粉等6种基质中10、20、50μg / kg 添加水平下的加标回收率范围为76.8％~100.3％，精密度范围为3.70％~12.6％。该方法无需使用对 LC-MS 联用仪容易造成污染的七氟正丁酸，且方法准确可靠，适用于大部分花粉基质的测定。
建立瞭花粉中鏈黴素（ streptomycin，STR）與雙氫鏈黴素（ dihydrostreptomycin，DHS）的高效液相色譜-串聯質譜（HPLC-MS / MS）檢測方法。樣品經提取液提取、三氯甲烷沉澱蛋白後，用 C18固相萃取柱進行富集淨化，採用 HPLC-MS / MS 對目標物進行定性確證和定量分析。在 Protemix WCX-NP5色譜柱（100 mm ×2.1 mm，5μm）上以5％（v / v）甲痠、20 mmol / L 醋痠銨和甲醇為流動相進行梯度洗脫分離；質譜採集模式為電噴霧正離子鑑測模式。鏈黴素和雙氫鏈黴素的檢齣限（以信譟比（ S / N）＝3計）均為5μg / kg，定量限（以 S / N ＝10計）均為10μg / kg；在10~200μg / L 的質量濃度範圍內呈現良好的線性關繫，相關繫數（ r）大于0.99。本底空白的鬆花粉、玉米花粉、茶花粉、葵花粉、油菜花粉、雜花粉等6種基質中10、20、50μg / kg 添加水平下的加標迴收率範圍為76.8％~100.3％，精密度範圍為3.70％~12.6％。該方法無需使用對 LC-MS 聯用儀容易造成汙染的七氟正丁痠，且方法準確可靠，適用于大部分花粉基質的測定。
건립료화분중련매소（ streptomycin，STR）여쌍경련매소（ dihydrostreptomycin，DHS）적고효액상색보-천련질보（HPLC-MS / MS）검측방법。양품경제취액제취、삼록갑완침정단백후，용 C18고상췌취주진행부집정화，채용 HPLC-MS / MS 대목표물진행정성학증화정량분석。재 Protemix WCX-NP5색보주（100 mm ×2.1 mm，5μm）상이5％（v / v）갑산、20 mmol / L 작산안화갑순위류동상진행제도세탈분리；질보채집모식위전분무정리자감측모식。련매소화쌍경련매소적검출한（이신조비（ S / N）＝3계）균위5μg / kg，정량한（이 S / N ＝10계）균위10μg / kg；재10~200μg / L 적질량농도범위내정현량호적선성관계，상관계수（ r）대우0.99。본저공백적송화분、옥미화분、다화분、규화분、유채화분、잡화분등6충기질중10、20、50μg / kg 첨가수평하적가표회수솔범위위76.8％~100.3％，정밀도범위위3.70％~12.6％。해방법무수사용대 LC-MS 련용의용역조성오염적칠불정정산，차방법준학가고，괄용우대부분화분기질적측정。
A method was established for the determination of streptomycin(STR)and dihydro-streptomycin(DHS)in pollens based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS / MS). The sample was extracted and cleaned-up by a C18 solid phase extraction cartridge. The separation was carried out on a Protemix WCX-NP5 column(100 mm ×2. 1 mm,5 μm)with a gradient elution using 5% ( v / v)formic acid,20 mmol / L ammonium acetate and methanol as mobile phases. The analysis of streptomycin and dihydrostreptomycin was performed under electrospray positive ionization mode. The limits of detection(LOD,S / N= 3)and limits of quantification( LOQ,S / N = 10)for the both were 5 μg / kg and 10 μg / kg, respectively. Good linearities(r ﹥0. 99)were achieved for the target compounds over the range of 10-200 μg / L. The recoveries at three spiked levels(10,20,50 μg / kg)in the blank matri-ces,such as pollen pini,corn pollen,camellia pollen,sunflower pollen,rape pollen and bee pollen,were from 76. 8% to 100. 3% with the relative standard deviations varied from 3. 70% to 12. 6% . The method is accurate,practical,and can be applied to most of the contaminated matrices. With this method,heptafluorobutyric acid is not required as mobile phase which is harmful to MS spectrometer.
