詳細(xì)介紹
HILIC技術(shù)越來(lái)越多的被用作HPLC方法開(kāi)發(fā)策略中的一部分。作為傳統(tǒng)反相色譜技術(shù)的補(bǔ)充,XBridge HILIC柱分離不僅保留高極性化合物,還能夠提供巨大的選擇性差異,獲得與反相分離時(shí)相反的洗脫順序。拓寬的PH使用范圍1-9,便于液相與質(zhì)譜方法開(kāi)發(fā)。HILIC保留機(jī)制是一個(gè)包含液液分配、離子交換與氫鍵的復(fù)雜過(guò)程,可增強(qiáng)極性分析物的保留。當(dāng)使用極性固定相,并且流動(dòng)相的乙腈濃度高于80%時(shí),化合物將會(huì)得到很好的保留。
為方法開(kāi)發(fā)提供互補(bǔ)選擇性
一種高效的方法開(kāi)發(fā)策略可同時(shí)使用XBridge HILIC色譜柱及XBridge 反相色譜柱來(lái)篩選分析物的選擇性及保留性。在一些情況 下,使用該方法可產(chǎn)生不同的洗脫順序或更佳的保留性,這 一特性有利于開(kāi)發(fā)極性分析物的分離方法。
增強(qiáng)極性堿性化合物的保留
HILIC保留機(jī)制是一個(gè)包含液液分配、離子交換與氫鍵的復(fù)雜 過(guò)程,可增強(qiáng)極性分析物的保留。當(dāng)使用極性固定相,并 且流動(dòng)相的乙腈濃度高于80%時(shí),化合物將會(huì)得到很好的保留。
提高質(zhì)譜分析的靈敏度
HILIC的使用已經(jīng)越來(lái)越普及,這主要是由于人們廣泛采用質(zhì) 譜儀作為檢測(cè)器,并且需要提高對(duì)極性分析物的定量靈敏 度。不同于使用高比例水相流動(dòng)相的反相分析方法,HILIC分 析方法中主要使用高比例乙腈流動(dòng)相。含有高比例有機(jī)相的 流動(dòng)相比較容易去溶劑化,從而增強(qiáng)離子強(qiáng)度及質(zhì)譜響應(yīng)。
人血漿高效液相色譜-串聯(lián)質(zhì)譜法的建立與評(píng)價(jià)
建立測(cè)定人血漿濃度的高效液相色譜-串聯(lián)質(zhì)譜法并評(píng)價(jià).方法 用甲醇蛋白質(zhì)沉淀法對(duì)血漿樣品預(yù)處理后,以乙腈-水(含200 mmol/L甲酸銨和0.1%甲酸)為流動(dòng)相梯度進(jìn)樣,流速為0.4 mL/min.通過(guò)色譜柱(Waters XBridge BEH HILIC,2.5 μm,2.1 mm×100 mm)分離樣品.以ESI正離子模式、多反應(yīng)離子監(jiān)測(cè)(MRM)模式監(jiān)測(cè)(m/z186.1→171.1作為定量離子對(duì)).用該方法檢測(cè)臨床患者血漿濃度,用ROC曲線評(píng)價(jià)血漿濃度和中毒嚴(yán)重指數(shù)(SIPP)對(duì)臨床結(jié)局的判斷價(jià)值.結(jié)果 血漿濃度在50~ 10 000 ng/mL時(shí),線性關(guān)系良好(R2=0.997),定量下限為50 ng/mL.低(100 ng/mL)、中(2 000 ng/mL)、高(8 000 ng/mL)3個(gè)濃度水平質(zhì)控品的不精密度均符合要求,且無(wú)基質(zhì)效應(yīng).處理后樣品室溫放置6h內(nèi)穩(wěn)定,樣本反復(fù)凍融3次對(duì)結(jié)果無(wú)影響.31例中毒患者SIPP為17.76(0.30~90.91)h·mg/L,死亡組SIPP高于存活組(P<0.05).SIPP的ROC曲線下面積為0.889,臨床臨界值為11.679 h·mg/L.結(jié)論 本法靈敏、準(zhǔn)確、快速、特異性好,適用于臨床檢測(cè)中毒患者.
XBridge BEH HILIC Column, XP Column, 130?, 2.5 µm, 2.1 mm X 150 mm, 3/pkg | 176002887 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 4.6 mm X 100 mm, 1/pkg | 186004440 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 4.6 mm X 150 mm, 1/pkg | 186004441 |
XBridge BEH HILIC Method Validation Kit, 130?, 2.5 µm, 2.1 mm X 150 mm, 3/pkg | 186006779 |
XBridge BEH HILIC Column, 130?, 5 µm, 2.1 mm X 30 mm, 1/pkg | 186004443 |
XBridge BEH HILIC Column, 130?, 5 µm, 2.1 mm X 50 mm, 1/pkg | 186004444 |
XBridge BEH HILIC Column, 130?, 5 µm, 2.1 mm X 150 mm, 1/pkg | 186004446 |
XBridge BEH HILIC Method Validation Kit, 130?, 2.5 µm, 3 mm X 100 mm, 3/pkg | 186006224 |
XBridge BEH HILIC Column, 130?, 5 µm, 2.1 mm X 100 mm, 1/pkg | 186004445 |
XBridge BEH HILIC Column, 130?, 5 µm, 3 mm X 100 mm, 1/pkg | 186004448 |
XBridge BEH HILIC Column, 130?, 5 µm, 3 mm X 50 mm, 1/pkg | 186004447 |
XBridge BEH HILIC Method Validation Kit, 130?, 2.5 µm, 2.1 mm X 50 mm, 3/pkg | 186006221 |
XBridge BEH HILIC Method Validation Kit, 130?, 2.5 µm, 2.1 mm X 100 mm, 3/pkg | 186006222 |
XBridge BEH HILIC Column, 130?, 5 µm, 4.6 mm X 250 mm, 1/pkg | 186004454 |
XBridge BEH HILIC Column, 130?, 5 µm, 4.6 mm X 100 mm, 1/pkg | 186004452 |
XBridge BEH HILIC Column, 130?, 5 µm, 4.6 mm X 150 mm, 1/pkg | 186004453 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 2.1 mm X 50 mm, 1/pkg | 186004432 |
XBridge BEH HILIC Column, 130?, 5 µm, 4.6 mm X 30 mm, 1/pkg | 186004450 |
XBridge BEH HILIC Column, 130?, 5 µm, 4.6 mm X 50 mm, 1/pkg | 186004451 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 2.1 mm X 30 mm, 1/pkg | 186004431 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 3 mm X 100 mm, 1/pkg | 186004436 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 3 mm X 50 mm, 1/pkg | 186004435 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 2.1 mm X 150 mm, 1/pkg | 186004434 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 4.6 mm X 50 mm, 1/pkg | 186004439 |
XBridge BEH HILIC Column, 130?, 3.5 µm, 4.6 mm X 30 mm, 1/pkg | 186004438 |
XBridge BEH HILIC VanGuard Cartridge, 130?, 5 µm, 3.9 mm X 5 mm, 3/pkg | 186007789 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 19 mm X 250 mm, 1/pkg | 186004730 |
XBridge BEH HILIC Prep Guard Cartridge, 130?, 5 µm, 30 mm X 10 mm, 1/pkg | 186006896 |
XBridge BEH HILIC Method Validation Kit, XP Column, 130?, 2.5 µm, 3 mm X 50 mm, 3/pkg | 186006223 |
XBridge BEH HILIC Method Validation Kit, 130?, 2.5 µm, 4.6 mm X 50 mm, 3/pkg | 186006225 |
XBridge BEH HILIC Method Validation Kit, 130?, 2.5 µm, 4.6 mm X 100 mm, 3/pkg | 186006226 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 50 mm X 50 mm, 1/pkg | 186004732 |
XBridge BEH HILIC VanGuard Cartridge, 130?, 3.5 µm, 3.9 mm X 5 mm, 3/pkg | 186007786 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 30 mm X 250 mm, 1/pkg | 186004731 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 50 mm X 150 mm, 1/pkg | 186004734 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 50 mm X 100 mm, 1/pkg | 186004733 |
XBridge BEH HILIC VanGuard Cartridge, 130?, 5 µm, 2.1 mm X 5 mm, 3/pkg | 186007787 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 50 mm X 250 mm, 1/pkg | 186004735 |
XBridge BEH HILIC XP Column, 130?, 2.5 µm, 2.1 mm X 100 mm, 3/pkg | 176002581 |
XBridge BEH HILIC VanGuard Cartridge, 130?, 3.5 µm, 2.1 mm X 5 mm, 3/pkg | 186007784 |
XBridge BEH HILIC Method Validation Kit, 130?, 2.5 µm, 3 mm X 150 mm, 3/pkg | 186006780 |
XBridge BEH HILIC Method Validation Kit, 130?, 2.5 µm, 4.6 mm X 150 mm, 3/pkg | 186006781 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 30 mm X 150 mm, 1/pkg | 186004729 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 30 mm X 100 mm, 1/pkg | 186004728 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 30 mm X 50 mm, 1/pkg | 186004727 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 19 mm X 150 mm, 1/pkg | 186004726 |
XBridge BEH HILIC OBD Prep Column, 130?, 5 µm, 19 mm X 100 mm, 1/pkg | 186004725 |
XBridge BEH HILIC Prep Guard Cartridge, 130?, 5 µm, 19 mm X 10 mm, 1/pkg | 186004723 |
XBridge BEH HILIC XP Column, 130?, 2.5 µm, 2.1 mm X 100 mm, 1/pkg | 186006079 |
XBridge BEH HILIC Prep Guard Cartridge, 130?, 5 µm, 10 mm X 10 mm, 1/pkg | 186004720 |