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Sulfur-fumigation has been forbidden in post-harvest handling of medicinal herbs.In present study, an HPLC-TQ-MS/MS method was developed for identification of sulfur-fumigated Radix Paeoniae Alba and its complex preparations.The purpose was achieved through simultaneously detecting paeoniflorin, the major component of Radix Paeoniae Alba, and paeoniflorin sulfonate, the artifact transformed from paeoniflorin during sulfur-fumigation of Radix Paeoniae Alba.Self-prepared sulfur-fumigated Radix Paeoniae Alba was used as reference herb to substitute paeoniflorin sulfonate reference compound which is commercially unavailable.