Supercritical fluid chromatography coupled to triple quadrupole mass spectrometry has been evaluated for pesticide residues in food. In order to check its advantages and limitations it was developed a method to identify and quantify 164 pesticides in three different matrices (tomato, orange and leek). A carbon dioxide gradient with methanol (containing 1 mM ammonium formate) was used allowing a flow rate of 1.5 mL/min that made the total run time of 12 min without any problem of overpressure. Addition of a post column flow 150 μL/min of Methanol with ammonium formate/formic acid was necessary to improve the ionization.

The matrix effect study revealed that the percentages of pesticides with irrelevant matrix effect (suppression lower than 20%) was 99% in tomato, 87% in orange and 62% in leek, whereas significant suppression (higher than 50%) was not found in tomato and only 1% of the compounds in orange and 3% in leek.These results compare favorably with that typically obtained in LC–MS/MS. The absence of water in the mobile phase, also provided some important advantages regarding LC–MS/MS as (i) higher retention of polar compounds in the column, which elute with high sensitivity and good peak shape and (ii) a general increase of the sensitivity of the analysis, consequence of the high ionization and ion extraction efficiency.

Pesticides evaluated were identified following the SANTE/11813/2017. At the spiking concentration of 5 μg/kg, 98% of the pesticides were identified in tomato, 98% in orange and 94% in leek, whereas for the concentration of 10 μg/kg all the compounds were identified in tomato and only spiromesifen was not identified in orange and leek. At the concentration of 20 μg/kg, spiromesifen was also identified in these two matrices. The linearity and reproducibility of the method were evaluated with results which guarantee high quality in the analytical measurements. Even though only 2 μL of final extract were injected, the sensitivity of the SFC method was enough to achieve stringent LOQs.Real samples, including 6 different fruits and vegetables, were analyzed by the SFC-MS/MS proposed method, the results being similar to those obtained by LC–MS/MS. The method was also applied to a proficiency test of fipronil in eggs with good results in all the cases.

Carbon dioxide as mobile phase with methanol as modifier can represent a good alternative to LC–MS/MS with reduction of matrix effects and shorter run times.

超临界流体色谱与三重四极杆质谱联用已对食品中的农药残留进行了评估。为了检查其优点和局限性，开发了一种在三种不同基质（西红柿，橙子和韭菜）中鉴定和定量164种农药的方法。使用含有甲醇（含1 mM甲酸铵）的二氧化碳梯度洗脱，流速为1.5 mL / min，使总运行时间为12分钟，而没有任何过压问题。为了提高电离度，必须在柱后添加150μL/ min的甲醇与甲酸铵/甲酸的溶液。

基质效应研究表明，与基质效应无关的农药（抑制率低于20％）的比例在番茄中为99％，在橙汁中为87％，在韭葱中为62％，而在番茄中未发现显着的抑制作用（高于50％）。番茄中只有1％的化合物为橙色，韭菜中的化合物为3％。这些结果与LC-MS / MS中通常获得的结果相比是有利的。流动相中没有水，这对于LC-MS / MS也提供了一些重要的优势，因为（i）极性化合物在色谱柱中的保留更高，洗脱时具有较高的灵敏度和良好的峰形，并且（ii）色谱柱的总体增加分析的敏感性，高电离和离子提取效率的结果。

根据SANTE / 11813/2017确定鉴定的农药。在加标浓度为5μg/ kg时，在番茄中鉴定出98％的农药，在橙汁中鉴定出98％的农药，在韭葱中鉴定出94％的农药，而在10μg/ kg的浓度下，在番茄中鉴定出所有化合物，仅螺索西芬未在橙色和韭葱中识别。当浓度为20μg/ kg时，在这两种基质中也鉴定出了spiromesifen。对方法的线性和重现性进行了评估，结果保证了分析测量的高质量。尽管仅注射了2μL最终提取物，但SFC方法的灵敏度仍足以实现严格的LOQs.SFC-MS / MS提出的方法对包括6种不同水果和蔬菜在内的实际样品进行了分析，结果相似通过LC-MS / MS获得的结果。

二氧化碳作为流动相，甲醇作为改性剂，可以减少基质效应并缩短运行时间，是LC-MS / MS的良好替代品。